Addition of Si-Containing Gases for Anisotropic Etching of III-V Materials in Chlorine-Based Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Gatilova, Lina; Bouchoule, Sophie; Patriarche, Gilles; Guilet, Stephane

2011-08-01

We discuss the possibility of obtaining high-aspect-ratio etching of InP materials in Cl2- and HBr-based inductively coupled plasmas (ICP) with the addition of Si-containing gases (SiH4 or SiCl4). A vertical and smooth etching profile is demonstrated in SiCl4/H2 plasma. The effect of adding of a small amount of SiH4 to a previously optimised Cl2/H2 chemistry is presented, and new SiH4/Cl2 and SiH4/HBr chemistries are proposed. Ex-situ energy-dispersive X-ray spectroscopy coupled to transmission electron microscopy (EDX-TEM) is used to analyze the composition of the thin passivation layer deposited on the etched sidewalls. We show that it consists of a Si-rich silicon oxide (Si/O˜1) in Cl2/H2/SiH4 chemistry, and is changed to nano-crystalline (nc-) Si in SiH4/Cl2 chemistry depending on the SiH4 percentage. Moreover, we show that deep anisotropic etching of InP independent of the electrode coverplate material can be obtained via a SiOx passivation mechanism with the addition of Si-containing gases.

Tissue response to peritoneal implants

NASA Technical Reports Server (NTRS)

Picha, G. J.

1980-01-01

Peritoneal implants were fabricated from poly 2-OH, ethyl methacrylate (HEMA), polyetherurethane (polytetramethylene glycol 1000 MW, 1,4 methylene disocynate, and ethyl diamine), and untreated and sputter treated polytetrafluoroethylene (PTFE). The sputter treated PTFE implants were produced by an 8 cm diameter argon ion source. The treated samples consisted of ion beam sputter polished samples, sputter etched samples (to produce a microscopic surface cone texture) and surface pitted samples (produced by ion beam sputtering to result in 50 microns wide by 100 microns deep square pits). These materials were implanted in rats for periods ranging from 30 minutes to 14 days. The results were evaluated with regard to cell type and attachment kinetics onto the different materials. Scanning electron microscopy and histological sections were also evaluated. In general the smooth hydrophobic surfaces attracted less cells than the ion etched PTFE or the HEMA samples. The ion etching was observed to enhance cell attachment, multinucleated giant cell (MNGC) formation, cell to cell contact, and fibrous capsule formation. The cell responsed in the case of ion etched PTFE to an altered surface morphology. However, equally interesting was the similar attachment kinetics of HEMA verses the ion etched PTFE. However, HEMA resulted in a markedly different response with no MNGC's formation, minimal to no capsule formation, and sample coverage by a uniform cell layer.

Micromorphological characterization of adhesive interface of sound dentin and total-etch and self-etch adhesives.

PubMed

Drobac, Milan; Stojanac, Igor; Ramić, Bojana; Premović, Milica; Petrović, Ljubomir

2015-01-01

The ultimate goal in restorative dentistry has always been to achieve strong and permanent bond between the dental tissues and filling materials. It is not easy to achieve this task because the bonding process is different for enamel and dentin-dentin is more humid and more organic than enamel. It is moisture and organic nature of dentin that make this hard tissue very complex to achieve adhesive bond. One of the first and most widely used tools for examining the adhesive bond between hard dental tissues and composite restorative materials is scanning electron microscopy. The aim of this study was scanning electron microscopy analyzes the interfacial micro morphology of total-etch and self-etch adhesives. Micro morphological characteristics of interface between total-etch adhesive (Prime & Bond NT) in combination with the corresponding composite (Ceram X Mono) were compared with those of self-etching adhesive (AdheSE One) in, combination with the corresponding composite (Tetric EvoCeram). The specimens were observed under 1000 x magnification of scanning electron microscopy (JEOL, JSM-6460 Low Vacuum). Measurement of the thickness of the hybrid layer of the examined com posite systems was performed with the software of the device used (NIH Image Analyser). Micromorphological analysis of interface showed that the hybrid layer in sound dentin was well formed, its average thickness being 2.68 microm, with a large number of resin tags and a large amount of lateral branches for specimens with a composite system Prime & Bond NT-Ceram X Mono. However, the specimens' with composite systems Adhese One-Tetric EvoCeram did not show the presence of hybrid layer and the resin tags were poorly represented. The results of this study suggest that total-etch adhesives bond better with sound dentin than self-etch adhesive.

Ion beam evaluation of silicon carbide membrane structures intended for particle detectors

NASA Astrophysics Data System (ADS)

Pallon, J.; Syväjärvi, M.; Wang, Q.; Yakimova, R.; Iakimov, T.; Elfman, M.; Kristiansson, P.; Nilsson, E. J. C.; Ros, L.

2016-03-01

Thin ion transmission detectors can be used as a part of a telescope detector for mass and energy identification but also as a pre-cell detector in a microbeam system for studies of biological effects from single ion hits on individual living cells. We investigated a structure of graphene on silicon carbide (SiC) with the purpose to explore a thin transmission detector with a very low noise level and having mechanical strength to act as a vacuum window. In order to reach very deep cavities in the SiC wafers for the preparation of the membrane in the detector, we have studied the Inductive Coupled Plasma technique to etch deep circular cavities in 325 μm prototype samples. By a special high temperature process the outermost layers of the etched SiC wafers were converted into a highly conductive graphitic layer. The produced cavities were characterized by electron microscopy, optical microscopy and proton energy loss measurements. The average membrane thickness was found to be less than 40 μm, however, with a slightly curved profile. Small spots representing much thinner membrane were also observed and might have an origin in crystal defects or impurities. Proton energy loss measurement (also called Scanning Transmission Ion Microscopy, STIM) is a well suited technique for this thickness range. This work presents the first steps of fabricating a membrane structure of SiC and graphene which may be an attractive approach as a detector due to the combined properties of SiC and graphene in a monolithic materials structure.

Stacking sequence and interlayer coupling in few-layer graphene revealed by in situ imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Zhu-Jun; Dong, Jichen; Cui, Yi

In the transition from graphene to graphite, the addition of each individual graphene layer modifies the electronic structure and produces a different material with unique properties. Controlled growth of few-layer graphene is therefore of fundamental interest and will provide access to materials with engineered electronic structure. Here we combine isothermal growth and etching experiments with in situ scanning electron microscopy to reveal the stacking sequence and interlayer coupling strength in few-layer graphene. The observed layer-dependent etching rates reveal the relative strength of the graphene graphene and graphene substrate interaction and the resulting mode of adlayer growth. Scanning tunnelling microscopy andmore » density functional theory calculations confirm a strong coupling between graphene edge atoms and platinum. Simulated etching confirms that etching can be viewed as reversed growth. This work demonstrates that real-time imaging under controlled atmosphere is a powerful method for designing synthesis protocols for sp2 carbon nanostructures in between graphene and graphite.« less

Stacking sequence and interlayer coupling in few-layer graphene revealed by in situ imaging

DOE PAGES

Wang, Zhu-Jun; Dong, Jichen; Cui, Yi; ...

2016-10-19

In the transition from graphene to graphite, the addition of each individual graphene layer modifies the electronic structure and produces a different material with unique properties. Controlled growth of few-layer graphene is therefore of fundamental interest and will provide access to materials with engineered electronic structure. Here we combine isothermal growth and etching experiments with in situ scanning electron microscopy to reveal the stacking sequence and interlayer coupling strength in few-layer graphene. The observed layer-dependent etching rates reveal the relative strength of the graphene graphene and graphene substrate interaction and the resulting mode of adlayer growth. Scanning tunnelling microscopy andmore » density functional theory calculations confirm a strong coupling between graphene edge atoms and platinum. Simulated etching confirms that etching can be viewed as reversed growth. This work demonstrates that real-time imaging under controlled atmosphere is a powerful method for designing synthesis protocols for sp2 carbon nanostructures in between graphene and graphite.« less

Stacking sequence and interlayer coupling in few-layer graphene revealed by in situ imaging

PubMed Central

Wang, Zhu-Jun; Dong, Jichen; Cui, Yi; Eres, Gyula; Timpe, Olaf; Fu, Qiang; Ding, Feng; Schloegl, R.; Willinger, Marc-Georg

2016-01-01

In the transition from graphene to graphite, the addition of each individual graphene layer modifies the electronic structure and produces a different material with unique properties. Controlled growth of few-layer graphene is therefore of fundamental interest and will provide access to materials with engineered electronic structure. Here we combine isothermal growth and etching experiments with in situ scanning electron microscopy to reveal the stacking sequence and interlayer coupling strength in few-layer graphene. The observed layer-dependent etching rates reveal the relative strength of the graphene–graphene and graphene–substrate interaction and the resulting mode of adlayer growth. Scanning tunnelling microscopy and density functional theory calculations confirm a strong coupling between graphene edge atoms and platinum. Simulated etching confirms that etching can be viewed as reversed growth. This work demonstrates that real-time imaging under controlled atmosphere is a powerful method for designing synthesis protocols for sp2 carbon nanostructures in between graphene and graphite. PMID:27759024

Defect structure of web silicon ribbon

NASA Technical Reports Server (NTRS)

Cunningham, B.; Strunk, H.; Ast, D.

1980-01-01

The results of a preliminary study of two dendritic web samples are presented. The structure and electrical activity of the defects in the silicon webs were studied. Optical microscopy of chemically etched specimens was used to determine dislocation densities. Samples were mechanically polished, then Secco etched for approximately 5 minutes. High voltage transmission electron microscopy was used to characterize the crystallographic nature of the defects.

New Deep Reactive Ion Etching Process Developed for the Microfabrication of Silicon Carbide

NASA Technical Reports Server (NTRS)

Evans, Laura J.; Beheim, Glenn M.

2005-01-01

Silicon carbide (SiC) is a promising material for harsh environment sensors and electronics because it can enable such devices to withstand high temperatures and corrosive environments. Microfabrication techniques have been studied extensively in an effort to obtain the same flexibility of machining SiC that is possible for the fabrication of silicon devices. Bulk micromachining using deep reactive ion etching (DRIE) is attractive because it allows the fabrication of microstructures with high aspect ratios (etch depth divided by lateral feature size) in single-crystal or polycrystalline wafers. Previously, the Sensors and Electronics Branch of the NASA Glenn Research Center developed a DRIE process for SiC using the etchant gases sulfur hexafluoride (SF6) and argon (Ar). This process provides an adequate etch rate of 0.2 m/min and yields a smooth surface at the etch bottom. However, the etch sidewalls are rougher than desired, as shown in the preceding photomicrograph. Furthermore, the resulting structures have sides that slope inwards, rather than being precisely vertical. A new DRIE process for SiC was developed at Glenn that produces smooth, vertical sidewalls, while maintaining an adequately high etch rate.

Comparative study of resist stabilization techniques for metal etch processing

NASA Astrophysics Data System (ADS)

Becker, Gerry; Ross, Matthew F.; Wong, Selmer S.; Minter, Jason P.; Marlowe, Trey; Livesay, William R.

1999-06-01

This study investigates resist stabilization techniques as they are applied to a metal etch application. The techniques that are compared are conventional deep-UV/thermal stabilization, or UV bake, and electron beam stabilization. The electron beam tool use din this study, an ElectronCure system from AlliedSignal Inc., ELectron Vision Group, utilizes a flood electron source and a non-thermal process. These stabilization techniques are compared with respect to a metal etch process. In this study, two types of resist are considered for stabilization and etch: a g/i-line resist, Shipley SPR-3012, and an advanced i-line, Shipley SPR 955- Cm. For each of these resist the effects of stabilization on resist features are evaluated by post-stabilization SEM analysis. Etch selectivity in all cases is evaluated by using a timed metal etch, and measuring resists remaining relative to total metal thickness etched. Etch selectivity is presented as a function of stabilization condition. Analyses of the effects of the type of stabilization on this method of selectivity measurement are also presented. SEM analysis was also performed on the features after a compete etch process, and is detailed as a function of stabilization condition. Post-etch cleaning is also an important factor impacted by pre-etch resist stabilization. Results of post- etch cleaning are presented for both stabilization methods. SEM inspection is also detailed for the metal features after resist removal processing.

Study of Etching Pits in a Large-grain Single Cell Bulk Niobium Cavity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Xin; Ciovati, Gianluigi; Reece, Charles E.

2009-11-01

Performance of SRF cavities are limited by non-linear localized effects. The variation of local material characters between "hot" and "cold" spots is thus of intense interest. Such locations were identified in a BCP-etched large-grain single-cell cavity and removed for examination by high resolution electron microscopy (SEM), electron-back scattering diffraction microscopy (EBSD), optical microscopy, and 3D profilometry. Pits with clearly discernable crystal facets were observed in both "hotspot" and "coldspot" specimens. The pits were found in-grain, at bi-crystal boundaries, and on tri-crystal junctions. They are interpreted as etch pits induced by surface crystal defects (e.g. dislocations). All "coldspots" examined had qualitativelymore » low density of etching pits or very shallow tri-crystal boundary junction. EBSD revealed crystal structure surrounding the pits via crystal phase orientation mapping, while 3D profilometry gave information on the depth and size of the pits. In addition, a survey of the samples by energy dispersive X-ray analysis (EDX) did not show any significant contamination of the samples surface.« less

Process margin enhancement for 0.25-μm metal etch process

NASA Astrophysics Data System (ADS)

Lee, Chung Y.; Ma, Wei Wen; Lim, Eng H.; Cheng, Alex T.; Joy, Raymond; Ross, Matthew F.; Wong, Selmer S.; Marlowe, Trey

2000-06-01

This study evaluates electron beam stabilization of UV6, a positive tone Deep-UV (DUV) resist from Shipley, for a 0.25 micrometer metal etch application. Results are compared between untreated resist and resist treated with different levels of electron beam stabilization. The electron beam processing was carried out in an ElectronCureTM flood electron beam exposure system from Honeywell International Inc., Electron Vision. The ElectronCureTM system utilizes a flood electron beam source which is larger in diameter than the substrate being processed, and is capable of variable energy so that the electron range is matched to the resist film thickness. Changes in the UV6 resist material as a result of the electron beam stabilization are monitored via spectroscopic ellipsometry for film thickness and index of refraction changes and FTIR for analysis of chemical changes. Thermal flow stability is evaluated by applying hot plate bakes of 150 degrees Celsius and 200 degrees Celsius, to patterned resist wafers with no treatment and with an electron beam dose level of 2000 (mu) C/cm2. A significant improvement in the thermal flow stability of the patterned UV6 resist features is achieved with the electron beam stabilization process. Etch process performance of the UV6 resist was evaluated by performing a metal pattern transfer process on wafers with untreated resist and comparing these with etch results on wafers with different levels of electron beam stabilization. The etch processing was carried out in an Applied Materials reactor with an etch chemistry including BCl3 and Cl2. All wafers were etched under the same conditions and the resist was treated after etch to prevent further erosion after etch but before SEM analysis. Post metal etch SEM cross-sections show the enhancement in etch resistance provided by the electron beam stabilization process. Enhanced process margin is achieved as a result of the improved etch resistance, and is observed in reduced resist side-wall angles after etch. Only a slight improvement is observed in the isolated to dense bias effects of the etch process. Improved CD control is also achieved by applying the electron beam process, as more consistent CDs are observed after etch.

Nano-textured high sensitivity ion sensitive field effect transistors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hajmirzaheydarali, M.; Sadeghipari, M.; Akbari, M.

2016-02-07

Nano-textured gate engineered ion sensitive field effect transistors (ISFETs), suitable for high sensitivity pH sensors, have been realized. Utilizing a mask-less deep reactive ion etching results in ultra-fine poly-Si features on the gate of ISFET devices where spacing of the order of 10 nm and less is achieved. Incorporation of these nano-sized features on the gate is responsible for high sensitivities up to 400 mV/pH in contrast to conventional planar structures. The fabrication process for this transistor is inexpensive, and it is fully compatible with standard complementary metal oxide semiconductor fabrication procedure. A theoretical modeling has also been presented to predict themore » extension of the diffuse layer into the electrolyte solution for highly featured structures and to correlate this extension with the high sensitivity of the device. The observed ultra-fine features by means of scanning electron microscopy and transmission electron microscopy tools corroborate the theoretical prediction.« less

Electron and Light Microscopy Techniques Suitable for Studying Fatigue Damage in a Crystallized Glass Ceramic

NASA Technical Reports Server (NTRS)

Harrell, Shelley; Zaretsky, Erwin V.

1961-01-01

The crystals of Pyroceram are randomly oriented and highly reflective so that standard microscopy techniques are not satisfactory for studying this material. Standard replicating procedures proved difficult to use. New microscopy techniques and procedures have therefore been developed. A method for locating, orienting, and identifying specific areas to be viewed with an electron microscope is described. This method not require any special equipment. Plastic replicas were found to be unsatisfactory because of their tendency to adhere to Pryoceram. This caused them to tear when released or resulted in artifacts. Preshadowed silicon monoxide replicas were satisfactory but required a releasing agent. A method of depositing the releasing agent is described. To polish specimens without evidence of fire-polishing, it was found necessary to use a vibratory polishing technique. Chrome oxide was used as the abrasive and either water or kerosene as the lubricant. Vibratory polishing is extremely slow, but surfaces so polished show no evidence of fire polishing, even when examined by electron microscopy. The most satisfactory etching process used for Pyroceram 9608 consisted of a primary etch of 5 milliliters of hydrochloric acid (concentrated), 5 milliliters of hydrogen fluoride (45 percent), and 45 milliliters of water, and a secondary etch with methyl alcohol replacing the water. Best results were obtained with total etching times from 25 to 30 seconds. Staining of the Pyroceram surface with a Sanford's marker was found to be an expedient way to reduce the glare of reflected light.

Surface micro-structuring of silicon by excimer-laser irradiation in reactive atmospheres

NASA Astrophysics Data System (ADS)

Pedraza, A. J.; Fowlkes, J. D.; Jesse, S.; Mao, C.; Lowndes, D. H.

2000-12-01

The formation mechanisms of cones and columns by pulsed-laser irradiation in reactive atmospheres were studied using scanning electron microscopy and profilometry. Deep etching takes place in SF6- and O2- rich atmospheres and consequently, silicon-containing molecules and clusters are released. Transport of silicon from the etched/ablated regions to the tip of columns and cones and to the side of the cones is required because both structures, columns and cones, protrude above the initial surface. The laser-induced micro-structure is influenced not only by the nature but also by the partial pressure of the reactive gas in the atmosphere. Irradiation in Ar following cone formation in SF6 produced no additional growth but rather melting and resolidification. Subsequent irradiation using again a SF6 atmosphere lead to cone restructuring and growth resumption. Thus the effects of etching plus re-deposition that produce column/cone formation and growth are clearly separated from the effects of just melting. On the other hand, irradiation continued in air after first performed in SF6 resulted in: (a) an intense etching of the cones and a tendency to transform them into columns; (b) growth of new columns on top of the existing cones and (c) filamentary nano-structures coating the sides of the columns and cones.

Catalyst free growth of CNTs by CVD on nanoscale rough surfaces of silicon substrates

NASA Astrophysics Data System (ADS)

Damodar, D.; Sahoo, R. K.; Jacob, C.

2013-06-01

Catalyst free growth of carbon nanotubes (CNT) has been achieved using atmospheric pressure chemical vapor deposition (APCVD) on surface modified Si(111) substrates. The effect of the substrate surface has been observed by partially etching with KOH (potassium hydroxide) solution which is an anisotropic etchant. Scanning electron microscopy (SEM) confirmed the formation of CNTs over most of the area of the substrate where substrates were anisotropically etched. Transmission electron microscopy (TEM) was used to observe the internal structure of the CNTs. Raman spectroscopy further confirmed the formation of the carbon nanostructures and also their graphitic crystallinity.

Elemental depth profiles and plasma etching rates of positive-tone electron beam resists after sequential infiltration synthesis of alumina

NASA Astrophysics Data System (ADS)

Ozaki, Yuki; Ito, Shunya; Hiroshiba, Nobuya; Nakamura, Takahiro; Nakagawa, Masaru

2018-06-01

By scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM–EDS), we investigated the elemental depth profiles of organic electron beam resist films after the sequential infiltration synthesis (SIS) of inorganic alumina. Although a 40-nm-thick poly(methyl methacrylate) (PMMA) film was entirely hybridized with alumina, an uneven distribution was observed near the interface between the substrate and the resist as well as near the resist surface. The uneven distribution was observed around the center of a 100-nm-thick PMMA film. The thicknesses of the PMMA and CSAR62 resist films decreased almost linearly as functions of plasma etching period. The comparison of etching rate among oxygen reactive ion etching, C3F8 reactive ion beam etching (RIBE), and Ar ion beam milling suggested that the SIS treatment enhanced the etching resistance of the electron beam resists to chemical reactions rather than to ion collisions. We proposed oxygen- and Ar-assisted C3F8 RIBE for the fabrication of silica imprint molds by electron beam lithography.

X-ray Reflectivity Study of a Highly Rough Surface: Si Nanowires Grown by Ag Nanoparticle Etching

NASA Astrophysics Data System (ADS)

Kremenak, Jesse; Arendse, Christopher; Cummings, Franscious; Chen, Yiyao; Miceli, Paul

Vertically oriented Si nanowires (SiNWs) formed by Ag-assisted wet chemical etching of a Si(100) substrate was studied by X-ray reflectivity (XRR) in combination with electron microscopy. Si(100) wafers coated with Ag nanoparticles, which serve as a catalyst, were etched for different durations in a HF/H2O2/DI-H2O solution. Because of the extreme roughness of these surfaces, there are challenges for using XRR methods in such systems. Therefore, significant attention is given to the analysis method of the XRR measurements. This sample-average information presents a valuable complement to electron microscopy studies, which focus on small sections of the sample. The present work shows-for the first time-the amount and distribution of Ag during the formation of SiNWs fabricated by Ag-assisted wet chemical etching, which is vital information for understanding the etching mechanisms. Support is gratefully acknowledged from the National Science Foundation (USA) - DGE1069091, the National Research Foundation (RSA) - TTK14052167658, 76568, 92520, and 93212; and the University of Missouri/University of Western Cape Linkage Program.

The effect of different chemical agents on human enamel: an atomic force and scanning electron microscopy study

NASA Astrophysics Data System (ADS)

Rominu, Roxana O.; Rominu, Mihai; Negrutiu, Meda Lavinia; Sinescu, Cosmin; Pop, Daniela; Petrescu, Emanuela

2010-12-01

PURPOSE: The goal of our study was to investigate the changes in enamel surface roughess induced by the application of different chemical substances by atomic force microscopy and scanning electron microscopy. METHOD: Five sound human first upper premolar teeth were chosen for the study. The buccal surface of each tooth was treated with a different chemical agent as follows: Sample 1 - 38% phosphoric acid etching (30s) , sample 2 - no surface treatment (control sample), 3 - bleaching with 37.5 % hydrogen peroxide (according to the manufacturer's instructions), 4 - conditioning with a self-etching primer (15 s), 5 - 9.6 % hydrofluoric acid etching (30s). All samples were investigated by atomic force microscopy in a non-contact mode and by scanning electron microscopy. Several images were obtained for each sample, showing evident differences regarding enamel surface morphology. The mean surface roughness and the mean square roughness were calculated and compared. RESULTS: All chemical substances led to an increased surface roughness. Phosphoric acid led to the highest roughness while the control sample showed the lowest. Hydrofluoric acid also led to an increase in surface roughness but its effects have yet to be investigated due to its potential toxicity. CONCLUSIONS: By treating the human enamel with the above mentioned chemical compounds a negative microretentive surface is obtained, with a morphology depending on the applied substance.

Surface morphology and dislocation characteristics near the surface of 4H-SiC wafer using multi-directional scanning transmission electron microscopy.

PubMed

Sato, Takahiro; Orai, Yoshihisa; Suzuki, Yuya; Ito, Hiroyuki; Isshiki, Toshiyuki; Fukui, Munetoshi; Nakamura, Kuniyasu; Schamp, C T

2017-10-01

To improve the reliability of silicon carbide (SiC) electronic power devices, the characteristics of various kinds of crystal defects should be precisely understood. Of particular importance is understanding the correlation between the surface morphology and the near surface dislocations. In order to analyze the dislocations near the surface of 4H-SiC wafers, a dislocation analysis protocol has been developed. This protocol consists of the following process: (1) inspection of surface defects using low energy scanning electron microscopy (LESEM), (2) identification of small and shallow etch pits using KOH low temperature etching, (3) classification of etch pits using LESEM, (4) specimen preparation of several hundred nanometer thick sample using the in-situ focused ion beam micro-sampling® technique, (5) crystallographic analysis using the selected diffraction mode of the scanning transmission electron microscope (STEM), and (6) determination of the Burgers vector using multi-directional STEM (MD-STEM). The results show a correlation between the triangular terrace shaped surface defects and an hexagonal etch pit arising from threading dislocations, linear shaped surface defects and elliptical shaped etch pits arising from basal plane dislocations. Through the observation of the sample from two orthogonal directions via the MD-STEM technique, a basal plane dislocation is found to dissociate into an extended dislocation bound by two partial dislocations. A protocol developed and presented in this paper enables one to correlate near surface defects of a 4H-SiC wafer with the root cause dislocations giving rise to those surface defects. © The Author 2017. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Electron beam induced etching of carbon nanotubes enhanced by secondary electrons in oxygen.

PubMed

Yoshida, Hideto; Tomita, Yuto; Soma, Kentaro; Takeda, Seiji

2017-05-12

Multi-walled carbon nanotubes (CNTs) are subjected to electron-beam-induced etching (EBIE) in oxygen. The EBIE process is observed in situ by environmental transmission electron microscopy. The partial pressure of oxygen (10 and 100 Pa), energy of the primary electrons (80 and 200 keV), and environment of the CNTs (suspended or supported on a silicon nitride membrane) are investigated as factors affecting the etching rate. The EBIE rate of CNTs was markedly promoted by the effects of secondary electrons that were emitted from a silicon nitride membrane under irradiation by primary electrons. Membrane supported CNTs can be cut by EBIE with a spatial accuracy better than 3 nm, and a nanogap of 2 nm can be successfully achieved between the ends of two suspended CNTs.

Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching.

PubMed

Nazarov, Denis V; Zemtsova, Elena G; Solokhin, Alexandr Yu; Valiev, Ruslan Z; Smirnov, Vladimir M

2017-01-13

In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed.

Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching

PubMed Central

Nazarov, Denis V.; Zemtsova, Elena G.; Solokhin, Alexandr Yu.; Valiev, Ruslan Z.; Smirnov, Vladimir M.

2017-01-01

In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed. PMID:28336849

Self-formation of a nanonet of fluorinated carbon nanowires on the Si surface by combined etching in fluorine-containing plasma

NASA Astrophysics Data System (ADS)

Amirov, I. I.; Gorlachev, E. S.; Mazaletskiy, L. A.; Izyumov, M. O.; Alov, N. V.

2018-03-01

In this work, we report a technique of the self-formation of a nanonet of fluorinated carbon nanowires on the Si surface using a combined etching in fluorine-containing C4F8/Ar and SF6 plasmas. Using scanning electron microscopy, atomic force microscopy and x-ray photoelectron spectroscopy, we show that after the etching of Si in the C4F8/Ar plasma, a fluorinated carbon film of nanometer-scale thickness is formed on its surface and its formation accelerates at elevated temperatures. After a subsequent short-term etching in the SF6 plasma, the film is modified into a nanonet of self-formed fluorinated carbon nanowires.

Single Etch-Pit Shape on Off-Angled 4H-SiC(0001) Si-Face Formed by Chlorine Trifluoride

NASA Astrophysics Data System (ADS)

Hatayama, Tomoaki; Tamura, Tetsuya; Yano, Hiroshi; Fuyuki, Takashi

2012-07-01

The etch pit shape of an off-angled 4H-SiC Si-face formed by chlorine trifluoride (ClF3) in nitrogen (N2) ambient has been studied. One type of etch pit with a crooked hexagonal shape was formed at an etching temperature below 500 °C. The angle of the etch pit measured from a cross-sectional atomic force microscopy image was about 10° from the [11bar 20] view. The dislocation type of the etch pit was discussed in relation to the etch pit shape and an electron-beam-induced current image.

Isotropically etched radial micropore for cell concentration, immobilization, and picodroplet generation.

PubMed

Perroud, Thomas D; Meagher, Robert J; Kanouff, Michael P; Renzi, Ronald F; Wu, Meiye; Singh, Anup K; Patel, Kamlesh D

2009-02-21

To enable several on-chip cell handling operations in a fused-silica substrate, small shallow micropores are radially embedded in larger deeper microchannels using an adaptation of single-level isotropic wet etching. By varying the distance between features on the photolithographic mask (mask distance), we can precisely control the overlap between two etch fronts and create a zero-thickness semi-elliptical micropore (e.g. 20 microm wide, 6 microm deep). Geometrical models derived from a hemispherical etch front show that micropore width and depth can be expressed as a function of mask distance and etch depth. These models are experimentally validated at different etch depths (25.03 and 29.78 microm) and for different configurations (point-to-point and point-to-edge). Good reproducibility confirms the validity of this approach to fabricate micropores with a desired size. To illustrate the wide range of cell handling operations enabled by micropores, we present three on-chip functionalities: continuous-flow particle concentration, immobilization of single cells, and picoliter droplet generation. (1) Using pressure differentials, particles are concentrated by removing the carrier fluid successively through a series of 44 shunts terminated by 31 microm wide, 5 microm deep micropores. Theoretical values for the concentration factor determined by a flow circuit model in conjunction with finite volume modeling are experimentally validated. (2) Flowing macrophages are individually trapped in 20 microm wide, 6 microm deep micropores by hydrodynamic confinement. The translocation of transcription factor NF-kappaB into the nucleus upon lipopolysaccharide stimulation is imaged by fluorescence microscopy. (3) Picoliter-sized droplets are generated at a 20 microm wide, 7 microm deep micropore T-junction in an oil stream for the encapsulation of individual E. coli bacteria cells.

Microscopic observations of X-ray and gamma-ray induced decomposition of ammonium perchlorate crystals

NASA Technical Reports Server (NTRS)

Herley, P. J.; Levy, P. W.

1972-01-01

The X-ray and gamma-ray induced decomposition of ammonium perchlorate was studied by optical, transmission, and scanning electron microscopy. This material is a commonly used oxidizer in solid propellents which could be employed in deep-space probes, and where they will be subjected to a variety of radiations for as long as ten years. In some respects the radiation-induced damage closely resembles the effects produced by thermal decomposition, but in other respects the results differ markedly. Similar radiation and thermal effects include the following: (1) irregular or ill-defined circular etch pits are formed in both cases; (2) approximately the same size pits are produced; (3) the pit density is similar; (4) the c face is considerably more reactive than the m face; and (5) most importantly, many of the etch pits are aligned in crystallographic directions which are the same for thermal or radiolytic decomposition. Thus, dislocations play an important role in the radiolytic decomposition process.

Solid-state transformation of Fe-rich intermetallic phases in Al–5.0Cu–0.6Mn squeeze cast alloy with variable Fe contents during solution heat treatment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Bo; School of Mechanical Engineering, Gui Zhou University, Guiyang 550000; Zhang, Weiwen, E-mail: mewzhang@scut.edu.cn

2015-06-15

The Al–5.0 wt.% Cu–0.6 wt.% Mn alloys with a variable Fe content were prepared by squeeze casting. Optical microscopy (OM), Deep etching technique, scanning electron microscopy(SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to examine the solid-state transformation of Fe-rich intermetallics during the solution heat treatment. The results showed that the Chinese script-like α-Fe, Al{sub 6}(FeMn) and needle-like Al{sub 3}(FeMn) phases transform to a new Cu-rich β-Fe (Al{sub 7}Cu{sub 2}(FeMn)) phase during solution heat treatment. The possible reaction and overall transformation kinetics of the solid-state phase transformation for the Fe-rich intermetallics were investigated. - Graphical abstract: Displaymore » Omitted - Highlights: • The α-Fe, Al{sub 6}(FeMn) and Al{sub 3}(FeMn) phases change to the β-Fe phases. • Possible reactions of Fe phases during solution heat treatment are discussed. • The overall fractional transformation rate follows an Avrami curve.« less

Electrical Current Leakage and Open-Core Threading Dislocations in AlGaN-Based Deep Ultraviolet Light-Emitting Diodes.

DOE PAGES

Moseley, Michael William; Allerman, Andrew A.; Crawford, Mary H.; ...

2014-08-04

Electrical current transport through leakage paths in AlGaN-based deep ultraviolet (DUV) lightemitting diodes (LEDs) and their effect on LED performance are investigated. Open-core threading dislocations, or nanopipes, are found to conduct current through nominally insulating Al0.7Ga0.3N layers and limit the performance of DUV-LEDs. A defect-sensitive phosphoric acid etch reveals these opencore threading dislocations in the form of large, micron-scale hexagonal etch pits visible with optical microscopy, while closed-core screw-, edge-, and mixed-type threading dislocations are represented by smaller and more numerous nanometer-scale pits visible by atomic-force microscopy. The electrical and optical performances of DUV-LEDs fabricated on similar Si-doped Al0.7Ga0.3N templatesmore » are found to have a strong correlation to the density of these nanopipes, despite their small fraction (<0.1% in this study) of the total density of threading dislocations.« less

Effects of a non-rinse conditioner on the enamel of primary teeth.

PubMed

Fava, Marcelo; Myaki, Silvio Issáo; Arana-Chavez, Victor Elias; Fava-de-Moraes, Flavio

2003-01-01

The aim of this in vitro study was to evaluate by scanning electron microscopy the morphological aspects of the enamel of primary teeth after etching with 36% phosphoric acid or a non-rinse conditioner. Ten naturally exfoliated anterior primary teeth were selected. The samples were subjected to prophylaxis with pumice paste and water using a low-speed hand piece. Etching was done on the buccal surface. Specimens were divided into 2 groups: G1 (n=10): etching with 36% phosphoric acid gel - Conditioner 36 (Dentsply) for 20 s, followed by water rinse for 15 s; G2 (n=10): etching with NRC - Non Rinse Conditioner (Dentsply) for 20 s, followed by air drying for 15 s. The samples were dehydrated, mounted on metal stubs, coated with gold and observed with Jeol JSM-6100 scanning electron microscope. Electron-micrographic analysis showed that both etching agents were effective for etching the enamel of primary teeth causing the formation of microporosities on the enamel surface, although the etching pattern was more effective with the use of 36% phosphoric acid gel.

Laser-etch patterning of metal oxide coated carbon nanotube 3D architectures.

PubMed

Aksu, Cemile; Ingram, Wade; Bradford, Philip D; Jur, Jesse S

2018-08-17

This paper describes a way to fabricate novel hybrid low density nanostructures containing both carbon nanotubes (CNTs) and ceramic nanotubes. Using atomic layer deposition, a thin film of aluminum oxide was conformally deposited on aligned multiwall CNT foams in which the CNTs make porous, three-dimensional interconnected networks. A CO 2 laser was used to etch pure alumina nanotube structures by burning out the underlying CNT substrate in discrete locations via the printed laser pattern. Structural and morphological transitions during the calcination process of aluminum oxide coated CNTs were investigated through in situ transmission electron microscopy and high-resolution scanning electron microscopy. Laser parameters were optimized to etch the CNT away (i.e. etching speed, power and focal length) while minimizing damage to the alumina nanotubes due to overheating. This study opens a new route for fabricating very low density three dimensionally patterned materials with areas of dissimilar materials and properties. To demonstrate the attributes of these structures, the etched areas were used toward anisotropic microfluidic liquid flow. The demonstration used the full thickness of the material to make complex pathways for the liquid flow in the structure. Through tuning of processing conditions, the alumina nanotube (etched) regions became hydrophilic while the bulk material remained hydrophobic and electrically conductive.

Vertical Si nanowire arrays fabricated by magnetically guided metal-assisted chemical etching

NASA Astrophysics Data System (ADS)

Chun, Dong Won; Kim, Tae Kyoung; Choi, Duyoung; Caldwell, Elizabeth; Kim, Young Jin; Paik, Jae Cheol; Jin, Sungho; Chen, Renkun

2016-11-01

In this work, vertically aligned Si nanowire arrays were fabricated by magnetically guided metal-assisted directional chemical etching. Using an anodized aluminum oxide template as a shadow mask, nanoscale Ni dot arrays were fabricated on an Si wafer to serve as a mask to protect the Si during the etching. For the magnetically guided chemical etching, we deposited a tri-layer metal catalyst (Au/Fe/Au) in a Swiss-cheese configuration and etched the sample under the magnetic field to improve the directionality of the Si nanowire etching and increase the etching rate along the vertical direction. After the etching, the nanowires were dried with minimal surface-tension-induced aggregation by utilizing a supercritical CO2 drying procedure. High-resolution transmission electron microscopy (HR-TEM) analysis confirmed the formation of single-crystal Si nanowires. The method developed here for producing vertically aligned Si nanowire arrays could find a wide range of applications in electrochemical and electronic devices.

New Technique for Fabrication of Scanning Single-Electron Transistor Microscopy Tips

NASA Astrophysics Data System (ADS)

Goodwin, Eric; Tessmer, Stuart

Fabrication of glass tips for Scanning Single-Electron Transistor Microscopy (SSETM) can be expensive, time consuming, and inconsistent. Various techniques have been tried, with varying levels of success in regards to cost and reproducibility. The main requirement for SSETM tips is to have a sharp tip ending in a micron-scale flat face to allow for deposition of a quantum dot. Drawing inspiration from methods used to create tips from optical fibers for Near-Field Scanning Optical Microscopes, our group has come up with a quick and cost effective process for creating SSETM tips. By utilizing hydrofluoric acid to etch the tips and oleic acid to guide the etch profile, optical fiber tips with appropriate shaping can be rapidly prepared. Once etched, electric leads are thermally evaporated onto each side of the tip, while an aluminum quantum dot is evaporated onto the face. Preliminary results using various metals, oxide layers, and lead thicknesses have proven promising.

In situ nanoscale observations of gypsum dissolution by digital holographic microscopy.

PubMed

Feng, Pan; Brand, Alexander S; Chen, Lei; Bullard, Jeffrey W

2017-06-01

Recent topography measurements of gypsum dissolution have not reported the absolute dissolution rates, but instead focus on the rates of formation and growth of etch pits. In this study, the in situ absolute retreat rates of gypsum (010) cleavage surfaces at etch pits, at cleavage steps, and at apparently defect-free portions of the surface are measured in flowing water by reflection digital holographic microscopy. Observations made on randomly sampled fields of view on seven different cleavage surfaces reveal a range of local dissolution rates, the local rate being determined by the topographical features at which material is removed. Four characteristic types of topographical activity are observed: 1) smooth regions, free of etch pits or other noticeable defects, where dissolution rates are relatively low; 2) shallow, wide etch pits bounded by faceted walls which grow gradually at rates somewhat greater than in smooth regions; 3) narrow, deep etch pits which form and grow throughout the observation period at rates that exceed those at the shallow etch pits; and 4) relatively few, submicrometer cleavage steps which move in a wave-like manner and yield local dissolution fluxes that are about five times greater than at etch pits. Molar dissolution rates at all topographical features except submicrometer steps can be aggregated into a continuous, mildly bimodal distribution with a mean of 3.0 µmolm -2 s -1 and a standard deviation of 0.7 µmolm -2 s -1 .

Some personal and historical notes on the utility of "deep-etch" electron microscopy for making cell structure/function correlations.

PubMed

Heuser, John E

2014-11-01

This brief essay talks up the advantages of metal replicas for electron microscopy and explains why they are still the best way to image frozen cells in the electron microscope. Then it explains our approach to freezing, namely the Van Harreveld trick of "slamming" living cells onto a supercold block of metal sprayed with liquid helium at -269ºC, and further talks up this slamming over the alternative of high-pressure freezing, which is much trickier but enjoys greater favor at the moment. This leads me to bemoan the fact that there are not more young investigators today who want to get their hands on electron microscopes and use our approach to get the most "true to life" views of cells out of them with a minimum of hassle. Finally, it ends with a few perspectives on my own career and concludes that, personally, I'm permanently stuck with the view of the "founding fathers" that cell ultrastructure will ultimately display and explain all of cell function, or as Palade said in his Nobel lecture,electron micrographs are "irresistible and half transparent … their meaning buried under only a few years of work," and "reasonable working hypotheses are already suggested by the ultrastructural organization itself." © 2014 Heuser.

Defect-selective dry etching for quick and easy probing of hexagonal boron nitride domains.

PubMed

Wu, Qinke; Lee, Joohyun; Park, Sangwoo; Woo, Hwi Je; Lee, Sungjoo; Song, Young Jae

2018-03-23

In this study, we demonstrate a new method to selectively etch the point defects or the boundaries of as-grown hexagonal boron nitride (hBN) films and flakes in situ on copper substrates using hydrogen and argon gases. The initial quality of the chemical vapor deposition-grown hBN films and flakes was confirmed by UV-vis absorption spectroscopy, atomic force microscopy, and transmission electron microscopy. Different gas flow ratios of Ar/H 2 were then employed to etch the same quality of samples and it was found that etching with hydrogen starts from the point defects and grows epitaxially, which helps in confirming crystalline orientations. However, etching with argon is sensitive to line defects (boundaries) and helps in visualizing the domain size. Finally, based on this defect-selective dry etching technique, it could be visualized that the domains of a polycrystalline hBN monolayer merged together with many parts, even with those that grew from a single nucleation seed.

Defect-selective dry etching for quick and easy probing of hexagonal boron nitride domains

NASA Astrophysics Data System (ADS)

Wu, Qinke; Lee, Joohyun; Park, Sangwoo; Woo, Hwi Je; Lee, Sungjoo; Song, Young Jae

2018-03-01

In this study, we demonstrate a new method to selectively etch the point defects or the boundaries of as-grown hexagonal boron nitride (hBN) films and flakes in situ on copper substrates using hydrogen and argon gases. The initial quality of the chemical vapor deposition-grown hBN films and flakes was confirmed by UV-vis absorption spectroscopy, atomic force microscopy, and transmission electron microscopy. Different gas flow ratios of Ar/H2 were then employed to etch the same quality of samples and it was found that etching with hydrogen starts from the point defects and grows epitaxially, which helps in confirming crystalline orientations. However, etching with argon is sensitive to line defects (boundaries) and helps in visualizing the domain size. Finally, based on this defect-selective dry etching technique, it could be visualized that the domains of a polycrystalline hBN monolayer merged together with many parts, even with those that grew from a single nucleation seed.

Effect of oxygen plasma etching on pore size-controlled 3D polycaprolactone scaffolds for enhancing the early new bone formation in rabbit calvaria.

PubMed

Kook, Min-Suk; Roh, Hee-Sang; Kim, Byung-Hoon

2018-05-02

This study was to investigate the effects of O 2 plasma-etching of the 3D polycaprolactone (PCL) scaffold surface on preosteoblast cell proliferation and differentiation, and early new bone formation. The PCL scaffolds were fabricated by 3D printing technique. After O 2 plasma treatment, surface characterizations were examined by scanning electron microscopy, atomic force microscopy, and contact angle. MTT assay was used to determine cell proliferation. To investigate the early new bone formation, rabbits were sacrificed at 2 weeks for histological analyses. As the O 2 plasma etching time is increased, roughness and hydrophilicity of the PCL scaffold surface increased. The cell proliferation and differentiation on plasma-etched samples was significantly increased than on untreated samples. At 2 weeks, early new bone formation in O 2 plasma-etched PCL scaffolds was the higher than that of untreated scaffolds. The O 2 plasma-etched PCL scaffolds showed increased preosteoblast differentiation as well as increased new bone formation.

Deep Etching Process Developed for the Fabrication of Silicon Carbide Microsystems

NASA Technical Reports Server (NTRS)

Beheim, Glenn M.

2000-01-01

Silicon carbide (SiC), because of its superior electrical and mechanical properties at elevated temperatures, is a nearly ideal material for the microminiature sensors and actuators that are used in harsh environments where temperatures may reach 600 C or greater. Deep etching using plasma methods is one of the key processes used to fabricate silicon microsystems for more benign environments, but SiC has proven to be a more difficult material to etch, and etch depths in SiC have been limited to several micrometers. Recently, the Sensors and Electronics Technology Branch at the NASA Glenn Research Center at Lewis Field developed a plasma etching process that was shown to be capable of etching SiC to a depth of 60 mm. Deep etching of SiC is achieved by inductive coupling of radiofrequency electrical energy to a sulfur hexafluoride (SF6) plasma to direct a high flux of energetic ions and reactive fluorine atoms to the SiC surface. The plasma etch is performed at a low pressure, 5 mtorr, which together with a high gas throughput, provides for rapid removal of the gaseous etch products. The lateral topology of the SiC microstructure is defined by a thin film of etch-resistant material, such as indium-tin-oxide, which is patterned using conventional photolithographic processes. Ions from the plasma bombard the exposed SiC surfaces and supply the energy needed to initiate a reaction between SiC and atomic fluorine. In the absence of ion bombardment, no reaction occurs, so surfaces perpendicular to the wafer surface (the etch sidewalls) are etched slowly, yielding the desired vertical sidewalls.

Formation of nanogaps in InAs nanowires by selectively etching embedded InP segments.

PubMed

Schukfeh, M I; Storm, K; Hansen, A; Thelander, C; Hinze, P; Beyer, A; Weimann, T; Samuelson, L; Tornow, M

2014-11-21

We present a method to fabricate nanometer scale gaps within InAs nanowires by selectively etching InAs/InP heterostructure nanowires. We used vapor-liquid-solid grown InAs nanowires with embedded InP segments of 10-60 nm length and developed an etching recipe to selectively remove the InP segment. A photo-assisted wet etching process in a mixture of acetic acid and hydrobromic acid gave high selectivity, with accurate removal of InP segments down to 20 nm, leaving the InAs wire largely unattacked, as verified using scanning electron and transmission electron microscopy. The obtained nanogaps in InAs wires have potential as semiconducting electrodes to investigate electronic transport in nanoscale objects. We demonstrate this functionality by dielectrophoretically trapping 30 nm diameter gold nanoparticles into the gap.

Vertically aligned cobalt hydroxide nano-flake coated electro-etched carbon fiber cloth electrodes for supercapacitors

NASA Astrophysics Data System (ADS)

Cheng, Qian; Tang, Jie; Zhang, Han; Qin, Lu-Chang

2014-11-01

We describe preparation and characterization of nanostructured electrodes using Co(OH)2 nano-flakes and carbon fiber cloth for supercapacitors. Nanostructured Co(OH)2 flakes are produced by electrodeposition and they are coated onto the electro-etched carbon fiber cloth. A highest specific capacitance of 3404.8 F g-1 and an area-normalized specific capacitance of 3.3 F cm-2 have been obtained from such electrodes. Morphology and structure of the nanostructured electrodes have been characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The electrochemical properties have been studied by cyclic voltammetry (CV), constant-current charge and discharge, electrochemical impedance spectroscopy (EIS), and long-time cycling.

Photoelectrochemical etching measurement of defect density in GaN grown by nanoheteroepitaxy

NASA Astrophysics Data System (ADS)

Ferdous, M. S.; Sun, X. Y.; Wang, X.; Fairchild, M. N.; Hersee, S. D.

2006-05-01

The density of dislocations in n-type GaN was measured by photoelectrochemical etching. A 10× reduction in dislocation density was observed compared to planar GaN grown at the same time. Cross-sectional transmission electron microscopy studies indicate that defect reduction is due to the mutual cancellation of dislocations with equal and opposite Burger's vectors. The nanoheteroepitaxy sample exhibited significantly higher photoluminescence intensity and higher electron mobility than the planar reference sample.

Sensors and Micromachined Devices for the Automotive and New Markets: The Delphi Delco Electronics MEMS Story.

NASA Astrophysics Data System (ADS)

Logsdon, James

2002-03-01

This presentation will provide a brief history of the development of MEMS products and technology, beginning with the manifold absolute pressure sensor in the late seventies through the current variety of Delphi Delco Electronics sensors available today. The technology development of micromachining from uncompensated P plus etch stops to deep reactive ion etching and the technology development of wafer level packaging from electrostatic bonding to glass frit sealing and silicon to silicon direct bonding will be reviewed.

Directional Etching of Silicon by Silver Nanostructures

NASA Astrophysics Data System (ADS)

Sharma, Pradeep; Wang, Yuh-Lin

2011-02-01

We report directional etching of nanostructures (nanochannels and nanotrenches) into the Si(100) substrates in aqueous HF and H2O2 solution by lithographically defined Ag patterns (nanoparticles, nanorods, and nanorings). The Effect of Ag/Si interface oxide on the directional etching has been studied by etching Ag/SiOx/Si samples of known interface oxide thickness. Based on high resolution transmission electron microscopy (HRTEM) imaging and TEM-energy dispersive X-ray (EDX) spectra of the Ag/Si interfaces, we propose that maintenance of the sub-nanometer oxide at the Ag/Si interfaces and Ag-Si interaction are the key factors which regulate the directional etching of Si.

Microshear bond strength of resin composite to teeth affected by molar hypomineralization using 2 adhesive systems.

PubMed

William, Vanessa; Burrow, Michael F; Palamara, Joseph E A; Messer, Louise B

2006-01-01

When restoring hypomineralized first permanent molars, placement of cavo-surface margins can be difficult to ascertain due to uncertainty of the bonding capability of the tooth surface. The purpose of this study was to investigate the adhesion of resin composite bonded to control and hypomineralized enamel with an all-etch single-bottle adhesive or self-etching primer adhesive. Specimens of control enamel (N=44) and hypomineralized enamel (N=45) had a 0.975-mm diameter composite rod (Filtek Supreme Universal Restorative) bonded with either 3M ESPE Single Bond or Clearfil SE Bond following manufacturers' instructions. Specimens were stressed in shear at 1 mm/min to failure (microshear bond strength). Etched enamel surfaces and enamel-adhesive interfaces were examined under scanning electron microscopy. The microshear bond strength (MPa) of resin composite bonded to hypomineralized enamel was significantly lower than for control enamel (3M ESPE Single Bond=7.08 +/- 4.90 vs 16.27 +/- 10.04; Clearfil SE Bond=10.39 +/- 7.56 vs 19.63 +/- 7.42; P=.001). Fractures were predominantly adhesive in control enamel and cohesive in hypomineralized enamel. Scotchbond etchant produced deep interprismatic and intercrystal porosity in control enamel and shallow etch patterns with minimal intercrystal porosity in hypomineralized enamel. Control enamel appeared almost unaffected by SE Primer; hypomineralized enamel showed shallow etching. The hypomineralized enamel-adhesive interface was porous with cracks in the enamel. The control enamel-adhesive interface displayed a hybrid layer of even thickness. The microshear bond strength of resin composite bonded to hypomineralized enamel was significantly lower than for control enamel. This was supported by differences seen in etch patterns and at the enamel-adhesive interface.

Acid-etching technique of non-decalcified bone samples for visualizing osteocyte-lacuno-canalicular network using scanning electron microscope.

PubMed

Lampi, Tiina; Dekker, Hannah; Ten Bruggenkate, Chris M; Schulten, Engelbert A J M; Mikkonen, Jopi J W; Koistinen, Arto; Kullaa, Arja M

2018-01-01

The aim of this study was to define the acid-etching technique for bone samples embedded in polymethyl metacrylate (PMMA) in order to visualize the osteocyte lacuno-canalicular network (LCN) for scanning electron microscopy (SEM). Human jaw bone tissue samples (N = 18) were collected from the study population consisting of patients having received dental implant surgery. After collection, the bone samples were fixed in 70% ethanol and non-decalcified samples embedded routinely into polymethyl metacrylate (PMMA). The PMMA embedded specimens were acid-etched in either 9 or 37% phosphoric acid (PA) and prepared for SEM for further analysis. PMMA embedded bone specimens acid-etched by 9% PA concentration accomplishes the most informative and favorable visualization of the LCN to be observed by SEM. Etching of PMMA embedded specimens is recommendable to start with 30 s or 40 s etching duration in order to find the proper etching duration for the samples examined. Visualizing osteocytes and LCN provides a tool to study bone structure that reflects changes in bone metabolism and diseases related to bone tissue. By proper etching protocol of non-decalcified and using scanning electron microscope it is possible to visualize the morphology of osteocytes and the network supporting vitality of bone tissue.

Role of strained nano-regions in the formation of subgrains in CaCu3Ti4O12

NASA Astrophysics Data System (ADS)

Fang, Tsang-Tse; Wang, Yong-Huei; Kuo, Jui-Chao

2011-07-01

Single-phase CaCu3Ti4O12 (CCTO) was synthesized by solid-state reaction. Electron backscatter diffraction, scanning electron microscopy, and atomic force microscopy were adopted to characterize the grain orientation, microstructure, and surface morphology of the CCTO samples with or without thermal etching. Bump strained nano-regions induced by the local compositional disorder at a nano-scale have been discovered, being the origin of the formation of subgrains in CCTO. The proposed mechanism for the formation of subgrains involves the formation of etched pits and subboundaries pertaining to the strained nano-regions rather than dislocation displacement. The dielectric response inside the grains of CCTO relevant to the strained nano-regions is also discussed.

Uniformity studies of inductively coupled plasma etching in fabrication of HgCdTe detector arrays

NASA Astrophysics Data System (ADS)

Bommena, R.; Velicu, S.; Boieriu, P.; Lee, T. S.; Grein, C. H.; Tedjojuwono, K. K.

2007-04-01

Inductively coupled plasma (ICP) chemistry based on a mixture of CH 4, Ar, and H II was investigated for the purpose of delineating HgCdTe mesa structures and vias typically used in the fabrication of second and third generation infrared photo detector arrays. We report on ICP etching uniformity results and correlate them with plasma controlling parameters (gas flow rates, total chamber pressure, ICP power and RF power). The etching rate and surface morphology of In-doped MWIR and LWIR HgCdTe showed distinct dependences on the plasma chemistry, total pressure and RF power. Contact stylus profilometry and cross-section scanning electron microscopy (SEM) were used to characterize the anisotropy of the etched profiles obtained after various processes and a standard deviation of 0.06 μm was obtained for etch depth on 128 x 128 format array vias. The surface morphology and the uniformity of the etched surfaces were studied by plan view SEM. Atomic force microscopy was used to make precise assessments of surface roughness.

Fabrication and etching processes of silicon-based PZT thin films

NASA Astrophysics Data System (ADS)

Zhao, Hongjin; Liu, Yanxiang; Liu, Jianshe; Ren, Tian-Ling; Liu, Li-Tian; Li, Zhijian

2001-09-01

Lead-zirconate-titanate (PZT) thin films on silicon were prepared by a sol-gel method. Phase characterization and crystal orientation of the films were investigated by x-ray diffraction analysis (XRD). It was shown that the PZT thin films had a perfect perovskite structure after annealed at a low temperature of 600 degrees C. PZT thin films were chemically etched using HCl/HF solution through typical semiconductor lithographic process, and the etching condition was optimized. The scanning electron microscopy results indicated that the PZT thin film etching problem was well solved for the applications of PZT thin film devices.

Composition and conductance distributions of single GeSi quantum rings studied by conductive atomic force microscopy combined with selective chemical etching.

PubMed

Lv, Y; Cui, J; Jiang, Z M; Yang, X J

2013-02-15

Atomic force microscopy imaging combined with selective chemical etching is employed to quantitatively investigate three-dimensional (3D) composition distributions of single GeSi quantum rings (QRs). In addition, the 3D quantitative composition distributions and the corresponding conductance distributions are simultaneously obtained on the same single GeSi QRs by conductive atomic force microscopy combined with selective chemical etching, allowing us to investigate the correlations between the conductance and composition distributions of single QRs. The results show that the QRs' central holes have higher Ge content, but exhibit lower conductance, indicating that the QRs' conductance distribution is not consistent with their composition distribution. By comparing the topography, composition and conductance profiles of the same single QRs before and after different etching processes, it is found that the conductance distributions of GeSi QRs do not vary with the change of composition distribution. Instead, the QRs' conductance distributions are found to be consistent with their topographic shapes, which can be supposed to be due to the shape determined electronic structures.

Composition, morphology and surface recombination rate of HCl-isopropanol treated and vacuum annealed InAs(1 1 1)A surfaces

NASA Astrophysics Data System (ADS)

Kesler, V. G.; Seleznev, V. A.; Kovchavtsev, A. P.; Guzev, A. A.

2010-05-01

X-ray photoelectron spectroscopy and atomic force microscopy were used to examine the chemical composition and surface morphology of InAs(1 1 1)A surface chemically etched in isopropanol-hydrochloric acid solution (HCl-iPA) and subsequently annealed in vacuum in the temperature range 200-500 °C. Etching for 2-30 min resulted in the formation of "pits" and "hillocks" on the sample surface, respectively 1-2 nm deep and high, with lateral dimensions 50-100 nm. The observed local formations, whose density was up to 3 × 10 8 cm -2, entirely vanished from the surface after the samples were vacuum-annealed at temperatures above 300 °C. Using a direct method, electron beam microanalysis, we have determined that the defects of the hillock type includes oxygen and excessive As, while the "pits" proved to be identical in their chemical composition to InAs. Vacuum anneals were found to cause a decrease in As surface concentration relative to In on InAs surface, with a concomitant rise of surface recombination rate.

Homogeneity of Ge-rich nanostructures as characterized by chemical etching and transmission electron microscopy.

PubMed

Bollani, Monica; Chrastina, Daniel; Montuori, Valeria; Terziotti, Daniela; Bonera, Emiliano; Vanacore, Giovanni M; Tagliaferri, Alberto; Sordan, Roman; Spinella, Corrado; Nicotra, Giuseppe

2012-02-03

The extension of SiGe technology towards new electronic and optoelectronic applications on the Si platform requires that Ge-rich nanostructures be obtained in a well-controlled manner. Ge deposition on Si substrates usually creates SiGe nanostructures with relatively low and inhomogeneous Ge content. We have realized SiGe nanostructures with a very high (up to 90%) Ge content. Using substrate patterning, a regular array of nanostructures is obtained. We report that electron microscopy reveals an abrupt change in Ge content of about 20% between the filled pit and the island, which has not been observed in other Ge island systems. Dislocations are mainly found within the filled pit and only rarely in the island. Selective chemical etching and electron energy-loss spectroscopy reveal that the island itself is homogeneous. These Ge-rich islands are possible candidates for electronic applications requiring locally induced stress, and optoelectronic applications which exploit the Ge-like band structure of Ge-rich SiGe.

Stereo imaging and cytocompatibility of a model dental implant surface formed by direct laser fabrication.

PubMed

Mangano, Carlo; Raspanti, Mario; Traini, Tonino; Piattelli, Adriano; Sammons, Rachel

2009-03-01

Direct laser fabrication (DLF) allows solids with complex geometry to be produced by sintering metal powder particles in a focused laser beam. In this study, 10 Ti6Al4V alloy model dental root implants were obtained by DLF, and surface characterization was carried out using stereo scanning electron microscopy to produce 3D reconstructions. The surfaces were extremely irregular, with approximately 100 microm deep, narrow intercommunicating crevices, shallow depressions and deep, rounded pits of widely variable shape and size, showing ample scope for interlocking with the host bone. Roughness parameters were as follows: R(t), 360.8 microm; R(z), 358.4 microm; R(a), 67.4 microm; and R(q), 78.0 microm. Disc specimens produced by DLF with an identically prepared surface were used for biocompatibility studies with rat calvarial osteoblasts: After 9 days, cells had attached and spread on the DLF surface, spanning across the crevices, and voids. Cell density was similar to that on a commercial rough microtextured surface but lower than on commercial smooth machined and smooth-textured grit-blasted, acid-etched surfaces. Human fibrin clot extension on the DLF surface was slightly improved by inorganic acid etching to increase the microroughness. With further refinements, DLF could be an economical means of manufacturing implants from titanium alloys. (c) 2008 Wiley Periodicals, Inc.

Stain-etched porous silicon nanostructures for multicrystalline silicon-based solar cells

NASA Astrophysics Data System (ADS)

Ben Rabha, M.; Hajji, M.; Belhadj Mohamed, S.; Hajjaji, A.; Gaidi, M.; Ezzaouia, H.; Bessais, B.

2012-02-01

In this paper, we study the optical, optoelectronic and photoluminescence properties of stain-etched porous silicon nanostructures obtained with different etching times. Special attention is given to the use of the stain-etched PS as an antireflection coating as well as for surface passivating capabilities. The surface morphology has been analyzed by scanning electron microscopy. The evolution of the Si-O and Si-H absorption bands was analyzed by Fourier transform infrared spectrometry before and after PS treatment. Results show that stain etching of the silicon surface drops the total reflectivity to about 7% in the 400-1100 nm wavelength range and the minority carrier lifetime enhances to about 48 μs.

Thermal oxidation and nitridation of Si nanowalls prepared by metal assisted chemical etching

NASA Astrophysics Data System (ADS)

Behera, Anil K.; Viswanath, R. N.; Lakshmanan, C.; Polaki, S. R.; Sarguna, R. M.; Mathews, Tom

2018-04-01

Silicon nanowalls with controlled orientation have been prepared using metal assisted chemical etching process. Thermal oxidation and nitridation processes have been carried out on the prepared silicon nanowalls under a control flow of oxygen/nitrogen gases independently at 1050°C for 900s. The morphology and structural properties of the as-prepared, oxidized and nitridated silicon nanowalls have been studied using the scanning electron microscopy and the Grazing incident X-ray diffraction techniques. The results obtained from the analysis of X-ray diffraction patterns and the microscopy images are discussed.

Nitride microlens arrays for blue and ultraviolet wavelength applications

NASA Astrophysics Data System (ADS)

Oder, T. N.; Shakya, J.; Lin, J. Y.; Jiang, H. X.

2003-05-01

Nitride microlens arrays with sizes as small as 10 μm in diameter have been fabricated on GaN and AlN epilayers using the method of photoresist reflow and inductively coupled plasma dry etching. The focal lengths of the microlenses varied from 7-30 μm as determined by theoretical fitting as well as by the near-field scanning optical microscopy measurement. Scanning electron and atomic force microscopies were used to obtain the surface profile of the microlenses which were found to match very well with hemispherical fitting and a surface roughness value around 1 nm was obtained. Nitride microlens arrays would be naturally chosen for green/blue to deep ultraviolet wavelength applications. In addition, nitride microlenses offer the possibility of integrating nitride-based microsize photonic devices as well as of coupling light into, out of, and between arrays of III-nitride emitters for other applications, such as spatially resolved fluorescence spectroscopy studies of biological and medical systems and optical links, thereby further expanding the applications of III nitrides.

AFM and SEM study of the effects of etching on IPS-Empress 2 TM dental ceramic

NASA Astrophysics Data System (ADS)

Luo, X.-P.; Silikas, N.; Allaf, M.; Wilson, N. H. F.; Watts, D. C.

2001-10-01

The aim of this study was to investigate the effects of increasing etching time on the surface of the new dental material, IPS-Empress 2 TM glass ceramic. Twenty one IPS-Empress 2 TM glass ceramic samples were made from IPS-Empress 2 TM ingots through lost-wax, hot-pressed ceramic fabrication technology. All samples were highly polished and cleaned ultrasonically for 5 min in acetone before and after etching with 9.6% hydrofluoric acid gel. The etching times were 0, 10, 20, 30, 60, 90 and 120 s respectively. Microstructure was analysed by scanning electron microscopy (SEM) and atomic force microscopy (AFM) was used to evaluate the surface roughness and topography. Observations with SEM showed that etching with hydrofluoric acid resulted in preferential dissolution of glass matrix, and that partially supported crystals within the glass matrix were lost with increasing etching time. AFM measurements indicated that etching increased the surface roughness of the glass-ceramic. A simple least-squares linear regression was used to establish a relationship between surface roughness parameters ( Ra, RMS), and etching time, for which r2>0.94. This study demonstrates the benefits of combining two microscopic methods for a better understanding of the surface. SEM showed the mode of action of hydrofluoric acid on the ceramic and AFM provided valuable data regarding the extent of surface degradation relative to etching time.

Bonding of universal adhesives to dentine--Old wine in new bottles?

PubMed

Chen, C; Niu, L-N; Xie, H; Zhang, Z-Y; Zhou, L-Q; Jiao, K; Chen, J-H; Pashley, D H; Tay, F R

2015-05-01

Multi-mode universal adhesives offer clinicians the choice of using the etch-and-rinse technique, selective enamel etch technique or self-etch technique to bond to tooth substrates. The present study examined the short-term in vitro performance of five universal adhesives bonded to human coronal dentine. Two hundred non-carious human third molars were assigned to five groups based on the type of the universal adhesives (Prime&Bond Elect, Scotchbond Universal, All-Bond Universal, Clearfil Universal Bond and Futurabond U). Two bonding modes (etch-and-rinse and self-etch) were employed for each adhesive group. Bonded specimens were stored in deionized water for 24h or underwent a 10,000-cycle thermocycling ageing process prior to testing (N=10). Microtensile bond testing (μTBS), transmission electron microscopy (TEM) of resin-dentine interfaces in non-thermocycled specimens and scanning electron microscopy (SEM) of tracer-infused water-rich zones within hybrid layers of thermocycled specimens were performed. Both adhesive type and testing condition (with/without thermocycling) have significant influences on μTBS. The use of each adhesive in either the etch-and-rinse or self-etch application mode did not result in significantly different μTBS to dentine. Hybrid layers created by these adhesives in the etch-and-rinse bonding mode and self-etch bonding mode were ∼5μm and ≤0.5μm thick respectively. Tracer-infused regions could be identified within the resin-dentine interface from all the specimens prepared. The increase in versatility of universal adhesives is not accompanied by technological advances for overcoming the challenges associated with previous generations of adhesives. Therapeutic adhesives with bio-protective and bio-promoting effects are still lacking in commercialized adhesives. Universal adhesives represent manufacturers' attempt to introduce versatility in product design via adaptation of a single-bottle self-etch adhesive for other application modes without compromising its bonding effectiveness. Published by Elsevier Ltd.

Electron-bombarded 〈110〉-oriented tungsten tips for stable tunneling electron emission

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamada, T. K.; Abe, T.; Nazriq, N. M. K.

A clean tungsten (W) tip apex with a robust atomic plane is required for producing a stable tunneling electron emission under strong electric fields. Because a tip apex fabricated from a wire by aqueous chemical etching is covered by impurity layers, heating treatment in ultra-high vacuum is experimentally known to be necessary. However, strong heating frequently melts the tip apex and causes unstable electron emissions. We investigated quantitatively the tip apex and found a useful method to prepare a tip with stable tunneling electron emissions by controlling electron-bombardment heating power. Careful characterizations of the tip structures were performed with combinationsmore » of using field emission I–V curves, scanning electron microscopy, X-ray diffraction (transmitted Debye-Scherrer and Laue) with micro-parabola capillary, field ion microscopy, and field emission microscopy. Tips were chemically etched from (1) polycrystalline W wires (grain size ∼1000 nm) and (2) long-time heated W wires (grain size larger than 1 mm). Heating by 10-40 W (10 s) was found to be good enough to remove oxide layers and produced stable electron emission; however, around 60 W (10 s) heating was threshold power to increase the tip radius, typically +10 ± 5 nm (onset of melting). Further, the grain size of ∼1000 nm was necessary to obtain a conical shape tip apex.« less

Preparation of scanning tunneling microscopy tips using pulsed alternating current etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Valencia, Victor A.; Thaker, Avesh A.; Derouin, Jonathan

An electrochemical method using pulsed alternating current etching (PACE) to produce atomically sharp scanning tunneling microscopy (STM) tips is presented. An Arduino Uno microcontroller was used to control the number and duration of the alternating current (AC) pulses, allowing for ready optimization of the procedures for both Pt:Ir and W tips using a single apparatus. W tips prepared using constant and pulsed AC power were compared. Tips fashioned using PACE were sharper than those etched with continuous AC power alone. Pt:Ir tips were prepared with an initial coarse etching stage using continuous AC power followed by fine etching using PACE.more » The number and potential of the finishing AC pulses was varied and scanning electron microscope imaging was used to compare the results. Finally, tip quality using the optimized procedures was verified by UHV-STM imaging. With PACE, at least 70% of the W tips and 80% of the Pt:Ir tips were of sufficiently high quality to obtain atomically resolved images of HOPG or Ni(111)« less

Caries-preventive effect of fissure sealant containing surface reaction-type pre-reacted glass ionomer filler and bonded by self-etching primer.

PubMed

Shimazu, Kisaki; Ogata, Kiyokazu; Karibe, Hiroyuki

2012-01-01

We aimed to evaluate the caries-preventive effect of a fissure sealant containing surface reaction-type pre-reacted glass ionomer (S-PRG) filler and bonded by self-etching primer versus those of 2 conventional resin-based sealants bonded by acid etching in terms of its impact on enamel demineralization and remineralization, enamel bond strength, and integrity of debonded enamel surfaces. Demineralization, remineralization, and bond strength on untreated enamel and enamel subsurface lesions of bovine incisors were assessed among the sealants by polarizing microscopy and microradiography; debonded enamel surfaces were examined by scanning electron microscopy. The conventional resin-based sealants bonded by acid etching caused surface defects on the enamel subsurface lesions and significantly increased the lesion depth (p = 0.014), indicative of enamel demineralization. However the S-PRG filler-containing sealant bonded by self-etching primer maintained the enamel surface integrity and inhibited enamel demineralization. No difference in bond strength on both untreated enamel and enamel subsurface lesions was noted among the sealants. An S-PRG filler-containing fissure sealant bonded by self-etching primer can prevent enamel demineralization, microleakage, and gaps without the tags created by acid etching regardless of the enamel condition. Such sealants are suitable for protecting the pits and fissures of immature permanent teeth.

Ultrananocrystalline diamond-coated nanoporous membranes support SK-N-SH neuroblastoma endothelial cell attachment.

PubMed

Yang, Kai-Hung; Nguyen, Alexander K; Goering, Peter L; Sumant, Anirudha V; Narayan, Roger J

2018-06-06

Ultrananocrystalline diamond (UNCD) has been demonstrated to have attractive features for biomedical applications and can be combined with nanoporous membranes for applications in drug delivery systems, biosensing, immunoisolation and single molecule analysis. In this study, free-standing nanoporous UNCD membranes with pore sizes of 100 or 400 nm were fabricated by directly depositing ultrathin UNCD films on nanoporous silicon nitride membranes and then etching away silicon nitride using reactive ion etching. Successful deposition of UNCD on the substrate with a novel process was confirmed with Raman spectroscopy, X-ray photoelectron spectroscopy, cross-section scanning electron microscopy (SEM) and transmission electron microscopy. Both sample types exhibited uniform geometry and maintained a clear hexagonal pore arrangement. Cellular attachment of SK-N-SH neuroblastoma endothelial cells was examined using confocal microscopy and SEM. Attachment of SK-N-SH cells onto UNCD membranes on both porous regions and solid surfaces was shown, indicating the potential use of UNCD membranes in biomedical applications such as biosensors and tissue engineering scaffolds.

Defect sensitive etching of hexagonal boron nitride single crystals

NASA Astrophysics Data System (ADS)

Edgar, J. H.; Liu, S.; Hoffman, T.; Zhang, Yichao; Twigg, M. E.; Bassim, Nabil D.; Liang, Shenglong; Khan, Neelam

2017-12-01

Defect sensitive etching (DSE) was developed to estimate the density of non-basal plane dislocations in hexagonal boron nitride (hBN) single crystals. The crystals employed in this study were precipitated by slowly cooling (2-4 °C/h) a nickel-chromium flux saturated with hBN from 1500 °C under 1 bar of flowing nitrogen. On the (0001) planes, hexagonal-shaped etch pits were formed by etching the crystals in a eutectic mixture of NaOH and KOH between 450 °C and 525 °C for 1-2 min. There were three types of pits: pointed bottom, flat bottom, and mixed shape pits. Cross-sectional transmission electron microscopy revealed that the pointed bottom etch pits examined were associated with threading dislocations. All of these dislocations had an a-type burgers vector (i.e., they were edge dislocations, since the line direction is perpendicular to the [ 2 11 ¯ 0 ]-type direction). The pit widths were much wider than the pit depths as measured by atomic force microscopy, indicating the lateral etch rate was much faster than the vertical etch rate. From an Arrhenius plot of the log of the etch rate versus the inverse temperature, the activation energy was approximately 60 kJ/mol. This work demonstrates that DSE is an effective method for locating threading dislocations in hBN and estimating their densities.

Fabrication of high aspect ratio TiO{sub 2} and Al{sub 2}O{sub 3} nanogratings by atomic layer deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shkondin, Evgeniy, E-mail: eves@fotonik.dtu.dk; Takayama, Osamu; Lavrinenko, Andrei V.

The authors report on the fabrication of TiO{sub 2} and Al{sub 2}O{sub 3} nanostructured gratings with an aspect ratio of up to 50. The gratings were made by a combination of atomic layer deposition (ALD) and dry etch techniques. The workflow included fabrication of a Si template using deep reactive ion etching followed by ALD of TiO{sub 2} or Al{sub 2}O{sub 3}. Then, the template was etched away using SF{sub 6} in an inductively coupled plasma tool, which resulted in the formation of isolated ALD coatings, thereby achieving high aspect ratio grating structures. SF{sub 6} plasma removes silicon selectively withoutmore » any observable influence on TiO{sub 2} or Al{sub 2}O{sub 3}, thus revealing high selectivity throughout the fabrication. Scanning electron microscopy was used to analyze every fabrication step. Due to nonreleased stress in the ALD coatings, the top parts of the gratings were observed to bend inward as the Si template was removed, thus resulting in a gradual change in the pitch value of the structures. The pitch on top of the gratings is 400 nm, and it gradually reduces to 200 nm at the bottom. The form of the bending can be reshaped by Ar{sup +} ion beam etching. The chemical purity of the ALD grown materials was analyzed by x-ray photoelectron spectroscopy. The approach presented opens the possibility to fabricate high quality optical metamaterials and functional nanostructures.« less

Dislocation substructure of mantle-derived olivine as revealed by selective chemical etching and transmission electron microscopy

USGS Publications Warehouse

Kirby, S.H.; Wegner, M.W.

1978-01-01

Cleaved and mechanically polished surfaces of olivine from peridotite xenoliths from San Carlos, Arizona, were chemically etched using the techniques of Wegner and Christie (1974). Dislocation etch pits are produced on all surface orientations and they tend to be preferentially aligned along the traces of subgrain boundaries, which are approximately parallel to (100), (010), and (001). Shallow channels were also produced on (010) surfaces and represent dislocations near the surface that are etched out along their lengths. The dislocation etch channel loops are often concentric, and emanate from (100) subgrain boundaries, which suggests that dislocation sources are in the boundaries. Data on subgrain misorientation and dislocation line orientation and arguments based on subgrain boundary energy minimization are used to characterize the dislocation structures of the subgrain boundaries. (010) subgrain boundaries are of the twist type, composed of networks of [100] and [001] screw dislocations. Both (100) and (001) subgrain boundaries are tilt walls composed of arrays of edge dislocation with Burgers vectors b=[100] and [001], respectively. The inferred slip systems are {001} ???100???, {100} ???001???, and {010} ???100??? in order of diminishing importance. Exploratory transmission electron microscopy is in accord with these identifications. The flow stresses associated with the development of the subgrain structure are estimated from the densities of free dislocations and from the subgrain dimensions. Inferred stresses range from 35 to 75 bars using the free dislocation densities and 20 to 100 bars using the subgrain sizes. ?? 1978 Springer-Verlag.

Effect of post-space treatment on retention of fiber posts in different root regions using two self-etching systems.

PubMed

Zhang, Ling; Huang, Li; Xiong, Yu; Fang, Ming; Chen, Ji-Hua; Ferrari, Marco

2008-06-01

The effect of post-space treatment on the retention of fiber posts in different root regions was evaluated using two self-etching systems. Post spaces were prepared in extracted premolars and then the root canals were subjected to one of the following post-space treatments: (i) water irrigation (control); (ii) etching with 35% phosphoric acid for 30 s; (iii) irrigation with 17% EDTA followed by 5.25% sodium hypochlorite (NaOCl); and (iv) ultrasonic agitation associated with 17% EDTA and 5.25% NaOCl irrigating solutions. The dentin surfaces were examined under scanning electron microscopy (SEM) after different post-space treatments. Fiber posts were then luted in the treated roots using resin cement with either Clearfil SE Bond or Clearfil DC Bond, and the thin-slice push-out test was performed. Scanning electron microscopy showed that all the post-space treatments tested were effective in removal of the smear layer of debris, or sealer/gutta-percha remnants, on the root canal. The apical push-out strength was affected by post-space treatment. Both 35% phosphoric acid etching and ultrasonic agitation in combination with EDTA/NaOCl irrigation improved the apical push-out strength of the fiber post, regardless of the type of self-etching system. A solo irrigation with an EDTA/NaOCl solution resulted in a lower apical push-out strength compared with the other two experimental groups.

Fabrication and optical characterization of imaging fiber-based nanoarrays.

PubMed

Tam, Jenny M; Song, Linan; Walt, David R

2005-09-15

In this paper, we present a technique for fabricating arrays containing a density at least 90 times higher than previously published. Specifically, we discuss the fabrication of two imaging fiber-based nanoarrays, one with 700nm features, another with 300nm features. With arrays containing up to 4.5x10(6) array elements/mm(2), these nanoarrays have an ultra-high packing density. A straightforward etching protocol is used to create nanowells into which beads can be deposited. These beads comprise the sensing elements of the nanoarray. Deposition of the nanobeads into the nanowells using two techniques is described. The surface characteristics of the etched arrays are examined with atomic force microscopy and scanning electron microscopy. Fluorescence microscopy was used to observe the arrays. The 300nm array features and the 500nm center-to-center distance approach the minimum feature sizes viewable using conventional light microscopy.

High strength fused silica flexures manufactured by femtosecond laser

NASA Astrophysics Data System (ADS)

Bellouard, Yves; Said, Ali A.; Dugan, Mark; Bado, Philippe

2009-02-01

Flexures are mechanical elements used in micro- and precision-engineering to precisely guide the motion of micro-parts. They consist of slender bodies that deform elastically upon the application of a force. Although counter-intuitive at first, fused silica is an attractive material for flexure. Pending that the machining process does not introduce surface flaws that would lead to catastrophic failure, the material has a theoretically high ultimate tensile strength of several GPa. We report on high-aspect ratio fused silica flexures manufactured by femtosecond laser combined with chemical etching. Notch-hinges with thickness as small as twenty microns and aspect ratios comparable to aspect ratios obtained by Deep- Reactive-Ion-Etching (DRIE) were fabricated and tested under different loading conditions. Multiple fracture tests were performed for various loading conditions and the cracks morphologies were analyzed using Scanning Electron Microscopy. The manufactured elements show outstanding mechanical properties with flexural strengths largely exceeding those obtained with other technologies and materials. Fused silica flexures offer a mean to combine integrated optics with micro-mechanics in a single monolithic substrate. Waveguides and mechanical elements can be combined in a monolithic devices opening new opportunities for integrated opto-mechatronics devices.

Selective etching of TiN over TaN and vice versa in chlorine-containing plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shin, Hyungjoo; Zhu Weiye; Liu Lei

2013-05-15

Selectivity of etching between physical vapor-deposited TiN and TaN was studied in chlorine-containing plasmas, under isotropic etching conditions. Etching rates for blanket films were measured in-situ using optical emission of the N{sub 2} (C{sup 3}{Pi}{sub u}{yields}B{sup 3}{Pi}{sub g}) bandhead at 337 nm to determine the etching time, and transmission electron microscopy to determine the starting film thickness. The etching selectivity in Cl{sub 2}/He or HCl/He plasmas was poor (<2:1). There was a window of very high selectivity of etching TiN over TaN by adding small amounts (<1%) of O{sub 2} in the Cl{sub 2}/He plasma. Reverse selectivity (10:1 of TaNmore » etching over TiN) was observed when adding small amounts of O{sub 2} to the HCl/He plasma. Results are explained on the basis of the volatility of plausible reaction products.« less

Nanostructured silicon membranes for control of molecular transport.

PubMed

Srijanto, Bernadeta R; Retterer, Scott T; Fowlkes, Jason D; Doktycz, Mitchel J

2010-11-01

A membrane that allows selective transport of molecular species requires precise engineering on the nanoscale. Membrane permeability can be tuned by controlling the physical structure and surface chemistry of the pores. Here, a combination of electron beam and optical lithography, along with cryogenic deep reactive ion etching, has been used to fabricate silicon membranes that are physically robust, have uniform pore sizes, and are directly integrated into a microfluidic network. Additional reductions in pore size were achieved using plasma enhanced chemical vapor deposition and atomic layer deposition of silicon dioxide to coat membrane surfaces. Cross sectioning of the membranes using focused ion beam milling was used to determine the physical shape of the membrane pores before and after coating. Functional characterization of the membranes was performed by using quantitative fluorescence microscopy to document the transport of molecular species across the membrane.

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

DOE PAGES

Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija; ...

2017-02-21

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less

Deep Reactive Ion Etching (DRIE) of High Aspect Ratio SiC Microstructures using a Time-Multiplexed Etch-Passivate Process

NASA Technical Reports Server (NTRS)

Evans, Laura J.; Beheim, Glenn M.

2006-01-01

High aspect ratio silicon carbide (SiC) microstructures are needed for microengines and other harsh environment micro-electro-mechanical systems (MEMS). Previously, deep reactive ion etching (DRIE) of low aspect ratio (AR less than or = 1) deep (greater than 100 micron) trenches in SiC has been reported. However, existing DRIE processes for SiC are not well-suited for definition of high aspect ratio features because such simple etch-only processes provide insufficient control over sidewall roughness and slope. Therefore, we have investigated the use of a time-multiplexed etch-passivate (TMEP) process, which alternates etching with polymer passivation of the etch sidewalls. An optimized TMEP process was used to etch high aspect ratio (AR greater than 5) deep (less than 100 micron) trenches in 6H-SiC. Power MEMS structures (micro turbine blades) in 6H-SiC were also fabricated.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Henry, Michael David; Young, Travis R.; Griffin, Ben

Here, this work reports the utilization of a recently developed film, ScAlN, as a silicon etch mask offering significant improvements in high etch selectivity to silicon. Utilization of ScAlN as a fluorine chemistry based deep reactive ion etch mask demonstrated etch selectivity at 23 550:1, four times better than AlN, 11 times better than Al 2O 3, and 148 times better than silicon dioxide with significantly less resputtering at high bias voltage than either Al 2O 3 or AlN. Ellipsometry film thickness measurements show less than 0.3 nm/min mask erosion rates for ScAlN. Micromasking of resputtered Al for Al 2Omore » 3, AlN, and ScAlN etch masks is also reported here, utilizing cross-sectional scanning electron microscope and confocal microscope roughness measurements. With lower etch bias, the reduced etch rate can be optimized to achieve a trench bottom surface roughness that is comparable to SiO 2 etch masks. Etch mask selectivity enabled by ScAlN is likely to make significant improvements in microelectromechanical systems, wafer level packaging, and plasma dicing of silicon.« less

Robust graphene membranes in a silicon carbide frame.

PubMed

Waldmann, Daniel; Butz, Benjamin; Bauer, Sebastian; Englert, Jan M; Jobst, Johannes; Ullmann, Konrad; Fromm, Felix; Ammon, Maximilian; Enzelberger, Michael; Hirsch, Andreas; Maier, Sabine; Schmuki, Patrik; Seyller, Thomas; Spiecker, Erdmann; Weber, Heiko B

2013-05-28

We present a fabrication process for freely suspended membranes consisting of bi- and trilayer graphene grown on silicon carbide. The procedure, involving photoelectrochemical etching, enables the simultaneous fabrication of hundreds of arbitrarily shaped membranes with an area up to 500 μm(2) and a yield of around 90%. Micro-Raman and atomic force microscopy measurements confirm that the graphene layer withstands the electrochemical etching and show that the membranes are virtually unstrained. The process delivers membranes with a cleanliness suited for high-resolution transmission electron microscopy (HRTEM) at atomic scale. The membrane, and its frame, is very robust with respect to thermal cycling above 1000 °C as well as harsh acidic or alkaline treatment.

Electrochemical fabrication of nanoporous copper films in choline chloride-urea deep eutectic solvent.

PubMed

Zhang, Q B; Abbott, Andrew P; Yang, C

2015-06-14

Nanoporous copper films were fabricated by a facile electrochemical alloying/dealloying process without the need of a template. A deep eutectic solvent made from choline chloride (ChCl) and urea was used with zinc oxide as the metal salt. Cyclic voltammetry was used to characterise the electrochemical reduction of zinc and follow Cu-Zn alloy formation on the copper substrate at elevated temperatures from 353 to 393 K. The alloy formation was confirmed by X-ray diffraction spectra. 3D, open and bicontinuous nanoporous copper films were obtained by in situ electrochemically etching (dealloying) of the zinc component in the Cu-Zn surface alloys at an appropriate potential (-0.4 V vs. Ag). This dealloying process was found to be highly temperature dependent and surface diffusion controlled, which involved the self-assembly of copper atoms at the alloy/electrolyte interface. Additionally, the effects of the deposition parameters, including deposition temperature, current density as well as total charge density on resulting the microstructure were investigated by scanning electron microscopy, and atomic force microscope.

The use of analytical surface tools in the fundamental study of wear. [atomic nature of wear

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1977-01-01

Various techniques and surface tools available for the study of the atomic nature of the wear of materials are reviewed These include chemical etching, x-ray diffraction, electron diffraction, scanning electron microscopy, low-energy electron diffraction, Auger emission spectroscopy analysis, electron spectroscopy for chemical analysis, field ion microscopy, and the atom probe. Properties of the surface and wear surface regions which affect wear, such as surface energy, crystal structure, crystallographic orientation, mode of dislocation behavior, and cohesive binding, are discussed. A number of mechanisms involved in the generation of wear particles are identified with the aid of the aforementioned tools.

Analysis of Multilayer Devices for Superconducting Electronics by High-Resolution Scanning Transmission Electron Microscopy and Energy Dispersive Spectroscopy

DOE PAGES

Missert, Nancy; Kotula, Paul G.; Rye, Michael; ...

2017-02-15

We used a focused ion beam to obtain cross-sectional specimens from both magnetic multilayer and Nb/Al-AlOx/Nb Josephson junction devices for characterization by scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX). An automated multivariate statistical analysis of the EDX spectral images produced chemically unique component images of individual layers within the multilayer structures. STEM imaging elucidated distinct variations in film morphology, interface quality, and/or etch artifacts that could be correlated to magnetic and/or electrical properties measured on the same devices.

ScAlN etch mask for highly selective silicon etching

DOE PAGES

Henry, Michael David; Young, Travis R.; Griffin, Ben

2017-09-08

Here, this work reports the utilization of a recently developed film, ScAlN, as a silicon etch mask offering significant improvements in high etch selectivity to silicon. Utilization of ScAlN as a fluorine chemistry based deep reactive ion etch mask demonstrated etch selectivity at 23 550:1, four times better than AlN, 11 times better than Al 2O 3, and 148 times better than silicon dioxide with significantly less resputtering at high bias voltage than either Al 2O 3 or AlN. Ellipsometry film thickness measurements show less than 0.3 nm/min mask erosion rates for ScAlN. Micromasking of resputtered Al for Al 2Omore » 3, AlN, and ScAlN etch masks is also reported here, utilizing cross-sectional scanning electron microscope and confocal microscope roughness measurements. With lower etch bias, the reduced etch rate can be optimized to achieve a trench bottom surface roughness that is comparable to SiO 2 etch masks. Etch mask selectivity enabled by ScAlN is likely to make significant improvements in microelectromechanical systems, wafer level packaging, and plasma dicing of silicon.« less

Anisotropic selective etching between SiGe and Si

NASA Astrophysics Data System (ADS)

Ishii, Yohei; Scott-McCabe, Ritchie; Yu, Alex; Okuma, Kazumasa; Maeda, Kenji; Sebastian, Joseph; Manos, Jim

2018-06-01

In Si/SiGe dual-channel FinFETs, it is necessary to simultaneously control the etched amounts of SiGe and Si. However, the SiGe etch rate is higher than the Si etch rate in not only halogen plasmas but also physical sputtering. In this study, we found that hydrogen plasma selectively etches Si over SiGe. The result shows that the selectivity of Si over SiGe can be up to 38 with increasing Ge concentration in SiGe. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) results indicate that hydrogen selectively bonds with Si rather than with Ge in SiGe. During the etching, hydrogen-induced Si surface segregation is also observed. It is also observed that the difference in etched amount between SiGe and Si can be controlled from positive to negative values even in Si/SiGe dual-channel fin patterning while maintaining the vertical profiles. Furthermore, no plasma-induced lattice damage was observed by transmission electron microscopy for both Si and SiGe fin sidewalls.

Defect characterization of silicon dendritic web ribbons

NASA Technical Reports Server (NTRS)

Cheng, L. J.

1985-01-01

Progress made in the study of defect characterization of silicon dendritic web ribbon is presented. Chemical etching is used combined with optical microscopy, as well as the electron beam induced current (EBIC) technique. Thermal annealing effect on carrier lifetime is examined.

Recovery of shallow junction GaAs solar cells damaged by electron irradiation

NASA Technical Reports Server (NTRS)

Walker, G. H.; Conway, E. J.

1978-01-01

Solar cells operated in space are subject to degradation from electron and proton radiation damage. It has been found that for deep junction p-GaAlAs/p-GaAs solar cells some of the electron radiation damage is removed by annealing the cells at 200 C. The reported investigation shows that shallow junction p-GaAlAs/p-GaAs/n-GaAs heteroface solar cells irradiated with 1 MeV electrons show a more complete recovery of short-circuit current than do the deep junction cells. The heteroface p-GaAlAs/p-GaAs/n-GaAs solar cells studied were fabricated using the etch-back epitaxy process.

Uniform lateral etching of tungsten in deep trenches utilizing reaction-limited NF3 plasma process

NASA Astrophysics Data System (ADS)

Kofuji, Naoyuki; Mori, Masahito; Nishida, Toshiaki

2017-06-01

The reaction-limited etching of tungsten (W) with NF3 plasma was performed in an attempt to achieve the uniform lateral etching of W in a deep trench, a capability required by manufacturing processes for three-dimensional NAND flash memory. Reaction-limited etching was found to be possible at high pressures without ion irradiation. An almost constant etching rate that showed no dependence on NF3 pressure was obtained. The effect of varying the wafer temperature was also examined. A higher wafer temperature reduced the threshold pressure for reaction-limited etching and also increased the etching rate in the reaction-limited region. Therefore, the control of the wafer temperature is crucial to controlling the etching amount by this method. We found that the uniform lateral etching of W was possible even in a deep trench where the F radical concentration was low.

Formation of nanostructured silicon surfaces by stain etching

PubMed Central

2014-01-01

In this work, we report the fabrication of ordered silicon structures by chemical etching of silicon in vanadium oxide (V2O5)/hydrofluoric acid (HF) solution. The effects of the different etching parameters including the solution concentration, temperature, and the presence of metal catalyst film deposition (Pd) on the morphologies and reflective properties of the etched Si surfaces were studied. Scanning electron microscopy (SEM) was carried out to explore the morphologies of the etched surfaces with and without the presence of catalyst. In this case, the attack on the surfaces with a palladium deposit begins by creating uniform circular pores on silicon in which we distinguish the formation of pyramidal structures of silicon. Fourier transform infrared spectroscopy (FTIR) demonstrates that the surfaces are H-terminated. A UV-Vis-NIR spectrophotometer was used to study the reflectance of the structures obtained. A reflectance of 2.21% from the etched Si surfaces in the wavelength range of 400 to 1,000 nm was obtained after 120 min of etching while it is of 4.33% from the Pd/Si surfaces etched for 15 min. PMID:25435830

Microtrenching-free two-step reactive ion etching of 4H-SiC using NF{sub 3}/HBr/O{sub 2} and Cl{sub 2}/O{sub 2}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tseng, Yuan-Hung, E-mail: yhtseng.ee99g@nctu.edu.tw; Tsui, Bing-Yue

2014-05-15

In this paper, the authors performed a reactive ion etch of a 4H-SiC substrate with a gas mixture of NF{sub 3}, HBr, and O{sub 2}, resulting in a microtrenching-free etch. The etch rate was 107.8 nm/min, and the selectivity over the oxide hard mask was ∼3.85. Cross-sectional scanning electron microscopy showed no microtrenching compared with etches using plasmas of NF{sub 3}, NF{sub 3}/HBr, and NF{sub 3}/O{sub 2}. Analyzing a variety of HBr/O{sub 2} mixing ratios, the authors discuss the additive effect of each gas and their respective potential mechanisms for alleviating microtrenching. To increase the radius of gyration of the bottommore » corners, they introduced a second etch step with Cl{sub 2}/O{sub 2} plasma. Fabricating simple metal-oxide-semiconductor capacitors on the two-step etched surface, the authors found that the electrical characteristics of the etched sample were nearly the same as the nonetched sample.« less

Porous silicon formation during Au-catalyzed etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Algasinger, Michael; Bernt, Maximilian; Koynov, Svetoslav

2014-04-28

The formation of “black” nano-textured Si during the Au-catalyzed wet-chemical etch process was investigated with respect to photovoltaic applications. Cross-sectional scanning electron microscopy (SEM) images recorded at different stages of the etch process exhibit an evolution of a two-layer structure, consisting of cone-like Si hillocks covered with a nano-porous Si (np-Si) layer. Optical measurements confirm the presence of a np-Si phase which appears after the first ∼10 s of the etch process and continuously increases with the etch time. Furthermore, the etch process was investigated on Si substrates with different doping levels (∼0.01–100 Ω cm). SEM images show a transition frommore » the two-layer morphology to a structure consisting entirely of np-Si for higher doping levels (<0.1 Ω cm). The experimental results are discussed on the basis of the model of a local electrochemical etch process. A better understanding of the metal-catalyzed etch process facilitates the fabrication of “black” Si on various Si substrates, which is of significant interest for photovoltaic applications.« less

Ultrastructure and Composition of the Nannochloropsis gaditana Cell Wall

PubMed Central

Scholz, Matthew J.; Weiss, Taylor L.; Jinkerson, Robert E.; Jing, Jia; Roth, Robyn; Goodenough, Ursula; Posewitz, Matthew C.

2014-01-01

Marine algae of the genus Nannochloropsis are promising producers of biofuel precursors and nutraceuticals and are also harvested commercially for aquaculture feed. We have used quick-freeze, deep-etch electron microscopy, Fourier transform infrared spectroscopy, and carbohydrate analyses to characterize the architecture of the Nannochloropsis gaditana (strain CCMP 526) cell wall, whose recalcitrance presents a significant barrier to biocommodity extraction. The data indicate a bilayer structure consisting of a cellulosic inner wall (∼75% of the mass balance) protected by an outer hydrophobic algaenan layer. Cellulase treatment of walls purified after cell lysis generates highly enriched algaenan preparations without using the harsh chemical treatments typically used in algaenan isolation and characterization. Nannochloropsis algaenan was determined to comprise long, straight-chain, saturated aliphatics with ether cross-links, which closely resembles the cutan of vascular plants. Chemical identification of >85% of the isolated cell wall mass is detailed, and genome analysis is used to identify candidate biosynthetic enzymes. PMID:25239976

Back-channel-etch amorphous indium-gallium-zinc oxide thin-film transistors: The impact of source/drain metal etch and final passivation

NASA Astrophysics Data System (ADS)

Nag, Manoj; Bhoolokam, Ajay; Steudel, Soeren; Chasin, Adrian; Myny, Kris; Maas, Joris; Groeseneken, Guido; Heremans, Paul

2014-11-01

We report on the impact of source/drain (S/D) metal (molybdenum) etch and the final passivation (SiO2) layer on the bias-stress stability of back-channel-etch (BCE) configuration based amorphous indium-gallium-zinc oxide (a-IGZO) thin-film transistors (TFTs). It is observed that the BCE configurations TFTs suffer poor bias-stability in comparison to etch-stop-layer (ESL) TFTs. By analysis with transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS), as well as by a comparative analysis of contacts formed by other metals, we infer that this poor bias-stability for BCE transistors having Mo S/D contacts is associated with contamination of the back channel interface, which occurs by Mo-containing deposits on the back channel during the final plasma process of the physical vapor deposited SiO2 passivation.

Micro Raman and photoluminescence spectroscopy of nano-porous n and p type GaN/sapphire(0001).

PubMed

Ingale, Alka; Pal, Suparna; Dixit, V K; Tiwari, Pragya

2007-06-01

Variation of depth within a single etching spot (3 mm circular diameter) was observed in nanoporous GaN epilayer obtained on photo-assisted electrochemical etching of n and p-type GaN. The different etching depth regions were studied using microRaman and PL(yellow region) for both n-type and p-type GaN. From Raman spectroscopy, we observed that increase in disorder is accompanied by stress relaxation, as depth of etching increases for n-type GaN epilayer. This is well corroborated with scanning electron microscopy results. Contrarily, for p-type GaN epilayer we found that for minimum etching depth, stress in epilayer increases with increase in disorder. This is understood with the fact that as grown p-type GaN is more disordered compared to n-type GaN due to heavy Mg doping and further disorder leads to lattice distortion leading to increase in stress.

High-aspect ratio micro- and nanostructures enabled by photo-electrochemical etching for sensing and energy harvesting applications

NASA Astrophysics Data System (ADS)

Alhalaili, Badriyah; Dryden, Daniel M.; Vidu, Ruxandra; Ghandiparsi, Soroush; Cansizoglu, Hilal; Gao, Yang; Saif Islam, M.

2018-03-01

Photo-electrochemical (PEC) etching can produce high-aspect ratio features, such as pillars and holes, with high anisotropy and selectivity, while avoiding the surface and sidewall damage caused by traditional deep reactive ion etching (DRIE) or inductively coupled plasma (ICP) RIE. Plasma-based techniques lead to the formation of dangling bonds, surface traps, carrier leakage paths, and recombination centers. In pursuit of effective PEC etching, we demonstrate an optical system using long wavelength (λ = 975 nm) infra-red (IR) illumination from a high-power laser (1-10 W) to control the PEC etching process in n-type silicon. The silicon wafer surface was patterned with notches through a lithography process and KOH etching. Then, PEC etching was introduced by illuminating the backside of the silicon wafer to enhance depth, resulting in high-aspect ratio structures. The effect of the PEC etching process was optimized by varying light intensities and electrolyte concentrations. This work was focused on determining and optimizing this PEC etching technique on silicon, with the goal of expanding the method to a variety of materials including GaN and SiC that are used in designing optoelectronic and electronic devices, sensors and energy harvesting devices.

Characterization of etch pits found on a large-grain bulk niobium superconducting radio-frequency resonant cavity

DOE PAGES

Zhao, Xin; Ciovati, G.; Bieler, T. R.

2010-12-15

The performance of superconducting radio-frequency (SRF) resonant cavities made of bulk niobium is limited by nonlinear localized effects. Surface analysis of regions of higher power dissipation is thus of intense interest. Such areas (referred to as “hotspots”) were identified in a large-grain single-cell cavity that had been buffered-chemical polished and dissected for examination by high resolution electron microscopy, electron backscattered diffraction microscopy (EBSD), and optical microscopy. Pits with clearly discernible crystal facets were observed in both “hotspot” and “coldspot” specimens. The pits were found in-grain, at bicrystal boundaries, and on tricrystal junctions. They are interpreted as etch pits induced bymore » crystal defects (e.g. dislocations). All coldspots examined had a qualitatively lower density of etch pits or relatively smooth tricrystal boundary junctions. EBSD mapping revealed the crystal orientation surrounding the pits. Locations with high pit density are correlated with higher mean values of the local average misorientation angle distributions, indicating a higher geometrically necessary dislocation content. In addition, a survey of the samples by energy dispersive x-ray analysis did not show any significant contamination of the samples’ surface. In conclusion, the local magnetic field enhancement produced by the sharp-edge features observed on the samples is not sufficient to explain the observed degradation of the cavity quality factor, which starts at peak surface magnetic field as low as 20 mT.« less

Viewing Integrated-Circuit Interconnections By SEM

NASA Technical Reports Server (NTRS)

Lawton, Russel A.; Gauldin, Robert E.; Ruiz, Ronald P.

1990-01-01

Back-scattering of energetic electrons reveals hidden metal layers. Experiment shows that with suitable operating adjustments, scanning electron microscopy (SEM) used to look for defects in aluminum interconnections in integrated circuits. Enables monitoring, in situ, of changes in defects caused by changes in temperature. Gives truer picture of defects, as etching can change stress field of metal-and-passivation pattern, causing changes in defects.

Chemical synthesis of oriented ferromagnetic LaSr-2 × 4 manganese oxide molecular sieve nanowires

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carretero-Genevrier, Adrián; Gazquez, Jaume; Magen, Cesar

2012-04-25

Here we report a chemical solution based method using nanoporous track-etched polymer templates for producing long and oriented LaSr-2 × 4 manganese oxide molecular sieve nanowires. Scanning transmission electron microscopy and electron energy loss spectroscopy analyses show that the nanowires are ferromagnetic at room temperature, single crystalline, epitaxially grown and self-aligned.

IDENTIFICATION OF A PROTEIN-CONTAINING ENAMEL MATRIX LAYER WHICH BRIDGES WITH THE DENTIN-ENAMEL JUNCTION OF ADULT HUMAN TEETH1

PubMed Central

Dusevich, Vladimir; Xu, Changqi; Wang, Yong; Walker, Mary P.; Gorski, Jeff P.

2012-01-01

Objective To investigate the ultrastructure and chemical composition of the dentin-enamel junction and adjacent enamel of minimally processed third molar tooth sections. Design Undecalcified human third molar erupted teeth were sectioned and etched with 4% EDTA or 37% phosphoric acid prior to visualization by scanning electron microscopy. Confocal Raman spectroscopy was carried out at 50 μm and more than 400 μm away from the dentin-enamel junction before and after mild etching. Results A novel organic protein-containing enamel matrix layer was identified for the first time using scanning electron microscopy of etched bucco-lingual sections of crowns. This layer resembles a three-dimensional fibrous meshwork that is visually distinct from enamel “tufts”. Previous studies have generally used harsher solvent conditions which likely removed this layer and precluded its prior characterization. The shape of the organic enamel layer generally reflected that of sheath regions of enamel rods and extended from the dentin-enamel junction about 100–400 μm into the cuspal enamel. This layer exhibited a Raman C—H stretching peak at ~2931 cm−1 characteristic of proteins and this signal correlated directly with the presence and location of the matrix layer as identified by scanning electron microscopy. Conclusions The enamel protein layer was most prominent close to the dentin-enamel junction and was largely absent in cuspal enamel >400 μm away from the dentin enamel junction. We hypothesize that this protein containing matrix layer could provide an important biomechanical linkage between the enamel and the dentin-enamel junction and by extension, with the dentin, of the adult tooth. PMID:22609172

Fabrication of volcano-shaped nano-patterned sapphire substrates using colloidal self-assembly and wet chemical etching.

PubMed

Geng, Chong; Zheng, Lu; Fang, Huajing; Yan, Qingfeng; Wei, Tongbo; Hao, Zhibiao; Wang, Xiaoqing; Shen, Dezhong

2013-08-23

Patterned sapphire substrates (PSS) have been widely used to enhance the light output power in GaN-based light emitting diodes. The shape and feature size of the pattern in a PSS affect its enhancement efficiency to a great degree. In this work we demonstrate the nanoscale fabrication of volcano-shaped PSS using a wet chemical etching approach in combination with a colloidal monolayer templating strategy. Detailed analysis by scanning electron microscopy reveals that the unique pattern shape is a result of the different corrosion-resistant abilities of silica masks of different effective heights during wet chemical etching. The formation of silica etching masks of different effective heights has been ascribed to the silica precursor solution in the interstice of the colloidal monolayer template being distributed unevenly after infiltration. In the subsequent wet chemical etching process, the active reaction sites altered as etching duration was prolonged, resulting in the formation of volcano-shaped nano-patterned sapphire substrates.

A Magnetorheological Polishing-Based Approach for Studying Precision Microground Surfaces of Tungsten Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shafrir, S.N.; Lambropoulos, J.C.; Jacobs, S.D.

2007-03-23

Surface features of tungsten carbide composites processed by bound abrasive deterministic microgrinding and magnetorheological finishing (MRF) were studied for five WC-Ni composites, including one binderless material. All the materials studied were nonmagnetic with different microstructures and mechanical properties. White-light interferometry, scanning electron microscopy, and atomic force microscopy were used to characterize the surfaces after various grinding steps, surface etching, and MRF spot-taking.

The origins and evolution of freeze-etch electron microscopy

PubMed Central

Heuser, John E.

2011-01-01

The introduction of the Balzers freeze-fracture machine by Moor in 1961 had a much greater impact on the advancement of electron microscopy than he could have imagined. Devised originally to circumvent the dangers of classical thin-section techniques, as well as to provide unique en face views of cell membranes, freeze-fracturing proved to be crucial for developing modern concepts of how biological membranes are organized and proved that membranes are bilayers of lipids within which proteins float and self-assemble. Later, when freeze-fracturing was combined with methods for freezing cells that avoided the fixation and cryoprotection steps that Moor still had to use to prepare the samples for his original invention, it became a means for capturing membrane dynamics on the millisecond time-scale, thus allowing a deeper understanding of the functions of biological membranes in living cells as well as their static ultrastructure. Finally, the realization that unfixed, non-cryoprotected samples could be deeply vacuum-etched or even freeze-dried after freeze-fracturing opened up a whole new way to image all the other molecular components of cells besides their membranes and also provided a powerful means to image the interactions of all the cytoplasmic components with the various membranes of the cell. The purpose of this review is to outline the history of these technical developments, to describe how they are being used in electron microscopy today and to suggest how they can be improved in order to further their utility for biological electron microscopy in the future. PMID:21844598

Comparison of photoemission characteristics between square and circular wire array GaAs photocathodes.

PubMed

Deng, Wenjuan; Peng, Xincun; Zou, Jijun; Wang, Weilu; Liu, Yun; Zhang, Tao; Zhang, Yijun; Zhang, Daoli

2017-11-10

Two types of negative electron affinity gallium arsenide (GaAs) wire array photocathodes were fabricated by reactive ion etching and inductively coupled plasma etching of bulk GaAs material. High density GaAs wire arrays with high periodicity and good morphology were verified using scanning electron microscopy, and photoluminescence spectra confirmed the wire arrays had good crystalline quality. Reflection spectra showed that circular GaAs wire arrays had superior light trapping compared with square ones. However, after Cs/O activation, the square GaAs wire array photocathodes showed enhanced spectral response. The integral sensitivity of the square wire array photocathodes was approximately 2.8 times that of the circular arrays.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Saxena, Shailendra K., E-mail: phd1211512@iiti.ac.in; Sahu, Gayatri; Sagdeo, Pankaj R.

Quantum confinement effect has been studied in cheese like silicon nano-structures (Ch-SiNS) fabricated by metal induced chemical etching using different etching times. Scanning electron microscopy is used for the morphological study of these Ch-SiNS. A visible photoluminescence (PL) emission is observed from the samples under UV excitation at room temperature due to quantum confinement effect. The average size of Silicon Nanostructures (SiNS) present in the samples has been estimated by bond polarizability model using Raman Spectroscopy from the red-shift observed from SiNSs as compared to its bulk counterpart. The sizes of SiNS present in the samples decreases as etching timemore » increase from 45 to 75 mintunes.« less

Effect of nanotechnology in self-etch bonding systems on the shear bond strength of stainless steel orthodontic brackets

PubMed Central

Hammad, Shaza M.; El-Wassefy, Noha; Maher, Ahmed; Fawakerji, Shafik M.

2017-01-01

ABSTRACT Objective: To evaluate the effect of silica dioxide (SiO2) nanofillers in different bonding systems on shear bond strength (SBS) and mode of failure of orthodontic brackets at two experimental times. Methods: Ninety-six intact premolars were divided into four groups: A) Conventional acid-etch and primer Transbond XT; B) Transbond Plus self-etch primer; and two self-etch bonding systems reinforced with silica dioxide nanofiller at different concentrations: C) Futurabond DC at 1%; D) Optibond All-in-One at 7%. Each group was allocated into two subgroups (n = 12) according to experimental time (12 and 24 hours). SBS test was performed using a universal testing machine. ARI scores were determined under a stereomicroscope. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to determine the size and distribution of nanofillers. One-way ANOVA was used to compare SBS followed by the post-hoc Tukey test. The chi-square test was used to evaluate ARI scores. Results: Mean SBS of Futurabond DC and Optibond All-in-One were significantly lower than conventional system, and there were no significant differences between means SBS obtained with all self-etch bonding systems used in the study. Lower ARI scores were found for Futurabond DC and Optibond All-in-One. There was no significant difference of SBS and ARI obtained at either time points for all bonding systems. Relative homogeneous distribution of the fillers was observed with the bonding systems. Conclusion: Two nanofilled systems revealed the lowest bond strengths, but still clinically acceptable and less adhesive was left on enamel. It is advisable not to load the brackets immediately to the maximum. PMID:28444018

Gold core@silver semishell Janus nanoparticles prepared by interfacial etching

NASA Astrophysics Data System (ADS)

Chen, Limei; Deming, Christopher P.; Peng, Yi; Hu, Peiguang; Stofan, Jake; Chen, Shaowei

2016-07-01

Gold core@silver semishell Janus nanoparticles were prepared by chemical etching of Au@Ag core-shell nanoparticles at the air/water interface. Au@Ag core-shell nanoparticles were synthesized by chemical deposition of a silver shell onto gold seed colloids followed by the self-assembly of 1-dodecanethiol onto the nanoparticle surface. The nanoparticles then formed a monolayer on the water surface of a Langmuir-Blodgett trough, and part of the silver shell was selectively etched away by the mixture of hydrogen peroxide and ammonia in the water subphase, where the etching was limited to the side of the nanoparticles that was in direct contact with water. The resulting Janus nanoparticles exhibited an asymmetrical distribution of silver on the surface of the gold cores, as manifested in transmission electron microscopy, UV-vis absorption, and X-ray photoelectron spectroscopy measurements. Interestingly, the Au@Ag semishell Janus nanoparticles exhibited enhanced electrocatalytic activity in oxygen reduction reactions, as compared to their Au@Ag and Ag@Au core-shell counterparts, likely due to a synergistic effect between the gold cores and silver semishells that optimized oxygen binding to the nanoparticle surface.Gold core@silver semishell Janus nanoparticles were prepared by chemical etching of Au@Ag core-shell nanoparticles at the air/water interface. Au@Ag core-shell nanoparticles were synthesized by chemical deposition of a silver shell onto gold seed colloids followed by the self-assembly of 1-dodecanethiol onto the nanoparticle surface. The nanoparticles then formed a monolayer on the water surface of a Langmuir-Blodgett trough, and part of the silver shell was selectively etched away by the mixture of hydrogen peroxide and ammonia in the water subphase, where the etching was limited to the side of the nanoparticles that was in direct contact with water. The resulting Janus nanoparticles exhibited an asymmetrical distribution of silver on the surface of the gold cores, as manifested in transmission electron microscopy, UV-vis absorption, and X-ray photoelectron spectroscopy measurements. Interestingly, the Au@Ag semishell Janus nanoparticles exhibited enhanced electrocatalytic activity in oxygen reduction reactions, as compared to their Au@Ag and Ag@Au core-shell counterparts, likely due to a synergistic effect between the gold cores and silver semishells that optimized oxygen binding to the nanoparticle surface. Electronic supplementary information (ESI) available: Additional TEM, UV-vis, XPS, and electrochemical data. See DOI: 10.1039/c6nr03368g

Correlation between dislocations and leakage current of p-n diodes on a free-standing GaN substrate

NASA Astrophysics Data System (ADS)

Usami, Shigeyoshi; Ando, Yuto; Tanaka, Atsushi; Nagamatsu, Kentaro; Deki, Manato; Kushimoto, Maki; Nitta, Shugo; Honda, Yoshio; Amano, Hiroshi; Sugawara, Yoshihiro; Yao, Yong-Zhao; Ishikawa, Yukari

2018-04-01

Dislocations that cause a reverse leakage current in vertical p-n diodes on a GaN free-standing substrate were investigated. Under a high reverse bias, dot-like leakage spots were observed using an emission microscope. Subsequent cathodoluminescence (CL) observations revealed that the leakage spots coincided with part of the CL dark spots, indicating that some types of dislocation cause reverse leakage. When etch pits were formed on the dislocations by KOH etching, three sizes of etch pits were obtained (large, medium, and small). Among these etch pits, only the medium pits coincided with leakage spots. Additionally, transmission electron microscopy observations revealed that pure screw dislocations are present under the leakage spots. The results revealed that 1c pure screw dislocations are related to the reverse leakage in vertical p-n diodes.

Nanosecond laser-induced back side wet etching of fused silica with a copper-based absorber liquid

NASA Astrophysics Data System (ADS)

Lorenz, Pierre; Zehnder, Sarah; Ehrhardt, Martin; Frost, Frank; Zimmer, Klaus; Schwaller, Patrick

2014-03-01

Cost-efficient machining of dielectric surfaces with high-precision and low-roughness for industrial applications is still challenging if using laser-patterning processes. Laser induced back side wet etching (LIBWE) using UV laser pulses with liquid heavy metals or aromatic hydrocarbons as absorber allows the fabrication of well-defined, nm precise, free-form surfaces with low surface roughness, e.g., needed for optical applications. The copper-sulphatebased absorber CuSO4/K-Na-Tartrate/NaOH/formaldehyde in water is used for laser-induced deposition of copper. If this absorber can also be used as precursor for laser-induced ablation, promising industrial applications combining surface structuring and deposition within the same setup could be possible. The etching results applying a KrF excimer (248 nm, 25 ns) and a Nd:YAG (1064 nm, 20 ns) laser are compared. The topography of the etched surfaces were analyzed by scanning electron microscopy (SEM), white light interferometry (WLI) as well as laser scanning microscopy (LSM). The chemical composition of the irradiated surface was studied by energy-dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FT-IR). For the discussion of the etching mechanism the laser-induced heating was simulated with finite element method (FEM). The results indicate that the UV and IR radiation allows micro structuring of fused silica with the copper-based absorber where the etching process can be explained by the laser-induced formation of a copper-based absorber layer.

Lead Pipe Scale Analysis Using Broad-Beam Argon Ion Milling to Elucidate Drinking Water Corrosion

EPA Science Inventory

Herein, we compared the characterization of lead pipe scale removed from a drinking water distribution system using two different cross section methods (conventional polishing and argon ion beam etching). The pipe scale solids were analyzed using scanning electron microscopy (SEM...

Nanogrids and Beehive-Like Nanostructures Formed by Plasma Etching the Self-Organized SiGe Islands

NASA Astrophysics Data System (ADS)

Chang, Yuan-Ming; Jian, Sheng-Rui; Juang, Jenh-Yih

2010-09-01

A lithography-free method for fabricating the nanogrids and quasi-beehive nanostructures on Si substrates is developed. It combines sequential treatments of thermal annealing with reactive ion etching (RIE) on SiGe thin films grown on (100)-Si substrates. The SiGe thin films deposited by ultrahigh vacuum chemical vapor deposition form self-assembled nanoislands via the strain-induced surface roughening (Asaro-Tiller-Grinfeld instability) during thermal annealing, which, in turn, serve as patterned sacrifice regions for subsequent RIE process carried out for fabricating nanogrids and beehive-like nanostructures on Si substrates. The scanning electron microscopy and atomic force microscopy observations confirmed that the resultant pattern of the obtained structures can be manipulated by tuning the treatment conditions, suggesting an interesting alternative route of producing self-organized nanostructures.

Permeability of Dental Adhesives – A SEM Assessment

PubMed Central

Malacarne-Zanon, Juliana; de Andrade e Silva, Safira M.; Wang, Linda; de Goes, Mario F.; Martins, Adriano Luis; Narvaes-Romani, Eliene O.; Anido-Anido, Andrea; Carrilho, Marcela R. O.

2010-01-01

Objectives: To morphologically evaluate the permeability of different commercial dental adhesives using scanning electron microscopy. Methods: Seven adhesive systems were evaluated: one three-step system (Scotchbond Multi-Purpose - MP); one two-step self-etching primer system (Clearfil SE Bond – SE); three two-step etch-and-rinse systems (Single Bond 2 – SB; Excite – EX; One-Step – OS); and two single-step self-etching adhesives (Adper Prompt – AP; One-Up Bond F – OU). The mixture of primer and bond agents of the Clearfil SE Bond system (SE-PB) was also tested. The adhesives were poured into a brass mold (5.8 mm x 0.8 mm) and light-cured for 80 s at 650 mW/cm2. After a 24 h desiccation process, the specimens were immersed in a 50% ammoniac silver nitrate solution for tracer permeation. Afterwards, they were sectioned in ultra-fine slices, carbon-coated, and analyzed under backscattered electrons in a scanning electron microscopy. Results: MP and SE showed slight and superficial tracer permeation. In EX, SB, and OS, permeation extended beyond the inner superficies of the specimens. SE-PB did not mix well, and most of the tracer was precipitated into the primer agent. In AP and OU, “water-trees” were observed all over the specimens. Conclusions: Different materials showed distinct permeability in aqueous solution. The extent of tracer permeation varied according to the composition of each material and it was more evident in the more hydrophilic and solvated ones. PMID:20922163

Capabilities of ICP-RIE cryogenic dry etching of silicon: review of exemplary microstructures

NASA Astrophysics Data System (ADS)

Sökmen, Ü.; Stranz, A.; Fündling, S.; Wehmann, H.-H.; Bandalo, V.; Bora, A.; Tornow, M.; Waag, A.; Peiner, E.

2009-10-01

Inductively coupled plasma (ICP) cryogenic dry etching was used to etch submicron pores, nano contact lines, submicron diameter pillars, thin and thick cantilevers, membrane structures and anisotropic deep structures with high aspect ratios in silicon for bio-nanoelectronics, optoelectronics and nano-micro electromechanical systems (NMEMS). The ICP cryogenic dry etching gives us the advantage of switching plasmas between etch rates of 13 nm min-1 and 4 µm min-1 for submicron pores and for membrane structures, respectively. A very thin photoresist mask can endure at -75 °C even during etching 70 µm deep for cantilevers and 300 µm deep for membrane structures. Coating the backsides of silicon membrane substrates with a thin photoresist film inhibited the lateral etching of cantilevers during their front release. Between -95 °C and -140 °C, we realized crystallographic-plane-dependent etching that creates facets only at the etch profile bottom. By varying the oxygen content and the process temperature, we achieved good control over the shape of the etched structures. The formation of black silicon during membrane etching down to 300 µm was delayed by reducing the oxygen content.

Anodic etching of GaN based film with a strong phase-separated InGaN/GaN layer: Mechanism and properties

NASA Astrophysics Data System (ADS)

Gao, Qingxue; Liu, Rong; Xiao, Hongdi; Cao, Dezhong; Liu, Jianqiang; Ma, Jin

2016-11-01

A strong phase-separated InGaN/GaN layer, which consists of multiple quantum wells (MQW) and superlattices (SL) layers and can produce a blue wavelength spectrum, has been grown on n-GaN thin film, and then fabricated into nanoporous structures by electrochemical etching method in oxalic acid. Scanning electron microscopy (SEM) technique reveals that the etching voltage of 8 V leads to a vertically aligned nanoporous structure, whereas the films etched at 15 V show branching pores within the n-GaN layer. Due to the low doping concentration of barriers (GaN layers) in the InGaN/GaN layer, we observed a record-low rate of etching (<100 nm/min) and nanopores which are mainly originated from the V-pits in the phase-separated layer. In addition, there exists a horizontal nanoporous structure at the interface between the phase-separated layer and the n-GaN layer, presumably resulting from the high transition of electrons between the barrier and the well (InGaN layer) at the interface. As compared to the as-grown MQW structure, the etched MQW structure exhibits a photoluminescence (PL) enhancement with a partial relaxation of compressive stress due to the increased light-extracting surface area and light-guiding effect. Such a compressive stress relaxation can be further confirmed by Raman spectra.

Reticulated shallow etch mesa isolation for controlling surface leakage in GaSb-based infrared detectors

NASA Astrophysics Data System (ADS)

Nolde, J. A.; Jackson, E. M.; Bennett, M. F.; Affouda, C. A.; Cleveland, E. R.; Canedy, C. L.; Vurgaftman, I.; Jernigan, G. G.; Meyer, J. R.; Aifer, E. H.

2017-07-01

Longwave infrared detectors using p-type absorbers composed of InAs-rich type-II superlattices (T2SLs) nearly always suffer from high surface currents due to carrier inversion on the etched sidewalls. Here, we demonstrate reticulated shallow etch mesa isolation (RSEMI): a structural method of reducing surface currents in longwave single-band and midwave/longwave dual-band detectors with p-type T2SL absorbers. By introducing a lateral shoulder to increase the separation between the n+ cathode and the inverted absorber surface, a substantial barrier to surface electron flow is formed. We demonstrate experimentally that the RSEMI process results in lower surface current, lower net dark current, much weaker dependence of the current on bias, and higher uniformity compared to mesas processed with a single deep etch. For the structure used, a shoulder width of 2 μm is sufficient to block surface currents.

Topography preserved microwave plasma etching for top-down layer engineering in MoS2 and other van der Waals materials.

PubMed

Varghese, Abin; Sharma, Chithra H; Thalakulam, Madhu

2017-03-17

A generic and universal layer engineering strategy for van der Waals (vW) materials, scalable and compatible with the current semiconductor technology, is of paramount importance in realizing all-two-dimensional logic circuits and to move beyond the silicon scaling limit. In this letter, we demonstrate a scalable and highly controllable microwave plasma based layer engineering strategy for MoS 2 and other vW materials. Using this technique we etch MoS 2 flakes layer-by-layer starting from an arbitrary thickness and area down to the mono- or the few-layer limit. From Raman spectroscopy, atomic force microscopy, photoluminescence spectroscopy, scanning electron microscopy and transmission electron microscopy, we confirm that the structural and morphological properties of the material have not been compromised. The process preserves the pre-etch layer topography and yields a smooth and pristine-like surface. We explore the electrical properties utilising a field effect transistor geometry and find that the mobility values of our samples are comparable to those of the pristine ones. The layer removal does not involve any reactive gasses or chemical reactions and relies on breaking the weak inter-layer vW interaction making it a generic technique for a wide spectrum of layered materials and heterostructures. We demonstrate the wide applicability of the technique by extending it to other systems such as graphene, h-BN and WSe 2 . In addition, using microwave plasma in combination with standard lithography, we illustrate a lateral patterning scheme making this process a potential candidate for large scale device fabrication in addition to layer engineering.

Effects of Etching Time and NaOH Concentration on the Production of Alumina Nanowires Using Porous Anodic Alumina Template

NASA Astrophysics Data System (ADS)

Sadeghpour-Motlagh, M.; Mokhtari-Zonouzi, K.; Aghajani, H.; Kakroudi, M. Ghassemi

2014-06-01

In this work, two-step anodizing of commercial aluminum foil in acid oxalic solution was applied for producing alumina film. Then the anodic alumina film was etched in sodium hydroxide (NaOH) solution resulting dense and aligned alumina nanowires. This procedure leads to splitting of alumina nanotubes. Subsequently nanowires are produced. The effects of NaOH solution concentration (0.2-1 mol/L) and etching time (60-300 s) at constant temperature on characteristic of nanotubes and produced nanowires were investigated using scanning electron microscopy. The results show that an increase in NaOH solution concentration increases the rate of nanowires production and in turn the manipulation process will be more specific.

Effect of deep cryogenic treatment on the formation of nano-sized carbides and the wear behavior of D2 tool steel

NASA Astrophysics Data System (ADS)

Amini, Kamran; Akhbarizadeh, Amin; Javadpour, Sirus

2012-09-01

The effect of deep cryogenic treatment on the microstructure, hardness, and wear behavior of D2 tool steel was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), hardness test, pin-on-disk wear test, and the reciprocating pin-on-flat wear test. The results show that deep cryogenic treatment eliminates retained austenite, makes a better carbide distribution, and increases the carbide content. Furthermore, some new nano-sized carbides form during the deep cryogenic treatment, thereby increasing the hardness and improving the wear behavior of the samples.

Techniques for the correction of topographical effects in scanning Auger electron microscopy

NASA Technical Reports Server (NTRS)

Prutton, M.; Larson, L. A.; Poppa, H.

1983-01-01

A number of ratioing methods for correcting Auger images and linescans for topographical contrast are tested using anisotropically etched silicon substrates covered with Au or Ag. Thirteen well-defined angles of incidence are present on each polyhedron produced on the Si by this etching. If N1 electrons are counted at the energy of an Auger peak and N2 are counted in the background above the peak, then N1, N1 - N2, (N1 - N2)/(N1 + N2) are measured and compared as methods of eliminating topographical contrast. The latter method gives the best compensation but can be further improved by using a measurement of the sample absorption current. Various other improvements are discussed.

Oxygen and nitrogen plasma etching of three-dimensional hydroxyapatite/chitosan scaffolds fabricated by additive manufacturing

NASA Astrophysics Data System (ADS)

Myung, Sung-Woon; Kim, Byung-Hoon

2016-01-01

Three-dimensional (3D) chitosan and hydroxyapatite (HAp)/chitosan (CH) scaffolds were fabricated by additive manufacturing, then their surfaces were etched with oxygen (O2) and nitrogen (N2) plasma. O2 and N2 plasma etching was performed to increase surface properties such as hydrophilicity, roughness, and surface chemistry on the scaffolds. After etching, hydroxyapatite was exposed on the surface of 3D HAp/CH scaffolds. The surface morphology and chemical properties were characterized by contact angle measurement, scanning electron microscopy, X-ray diffraction, and attenuated total reflection Fourier infrared spectroscopy. The cell viability of 3D chitosan scaffolds was examined by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. The differentiation of preosteoblast cells was evaluated by alkaline phosphatase assay. The cell viability was improved by O2 and N2 plasma etching of 3D chitosan scaffolds. The present fabrication process for 3D scaffolds might be applied to a potential tool for preparing biocompatible scaffolds.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Comparison between universal adhesives and two-step self-etch adhesives in terms of dentin bond fatigue durability in self-etch mode.

PubMed

Tsujimoto, Akimasa; Barkmeier, Wayne W; Takamizawa, Toshiki; Watanabe, Hidehiko; Johnson, William W; Latta, Mark A; Miyazaki, Masashi

2017-06-01

This aim of this study was to compare universal adhesives and two-step self-etch adhesives in terms of dentin bond fatigue durability in self-etch mode. Three universal adhesives - Clearfil Universal, G-Premio Bond, and Scotchbond Universal Adhesive - and three-two-step self-etch adhesives - Clearfil SE Bond, Clearfil SE Bond 2, and OptiBond XTR - were used. The initial shear bond strength and shear fatigue strength of resin composite bonded to adhesive on dentin in self-etch mode were determined. Scanning electron microscopy observations of fracture surfaces after bond strength tests were also made. The initial shear bond strength of universal adhesives was material dependent, unlike that of two-step self-etch adhesives. The shear fatigue strength of Scotchbond Universal Adhesive was not significantly different from that of two-step self-etch adhesives, unlike the other universal adhesives. The shear fatigue strength of universal adhesives differed depending on the type of adhesive, unlike those of two-step self-etch adhesives. The results of this study encourage the continued use of two-step self-etch adhesive over some universal adhesives but suggest that changes to the composition of universal adhesives may lead to a dentin bond fatigue durability similar to that of two-step self-etch adhesives. © 2017 Eur J Oral Sci.

Photocatalytic Active Bismuth Fluoride/Oxyfluoride Surface Crystallized 2Bi2O3-B2O3 Glass-Ceramics

NASA Astrophysics Data System (ADS)

Sharma, Sumeet Kumar; Singh, V. P.; Chauhan, Vishal S.; Kushwaha, H. S.; Vaish, Rahul

2018-03-01

The present article deals with 2Bi2O3-B2O3 (BBO) glass whose photocatalytic activity has been enhanced by the method of wet etching using an aqueous solution of hydrofluoric acid (HF). X-ray diffraction of the samples reveals that etching with an aqueous solution of HF leads to the formation of BiF3 and BiO0.1F2.8 phases. Surface morphology obtained from scanning electron microscopy show granular and plate-like morphology on the etched glass samples. Rhodamine 6G (Rh 6G) has been used to investigate the photocatalytic activity of the as-quenched and etched glasses. Enhanced visible light-driven photocatalytic activity was observed in HF etched glass-ceramics compared to the as-quenched BBO glass. Contact angle of the as-quenched glass was 90.2°, which decreases up to 20.02° with an increase in concentration of HF in the etching solution. Enhanced photocatalytic activity and increase in the hydrophilic nature suggests the efficient treatment of water pollutants by using the prepared surface crystallized glass-ceramics.

In-chip microstructures and photonic devices fabricated by nonlinear laser lithography deep inside silicon

PubMed Central

Makey, Ghaith; Elahi, Parviz; Çolakoğlu, Tahir; Ergeçen, Emre; Yavuz, Özgün; Hübner, René; Borra, Mona Zolfaghari; Pavlov, Ihor; Bek, Alpan; Turan, Raşit; Kesim, Denizhan Koray; Tozburun, Serhat; Ilday, Serim; Ilday, F. Ömer

2017-01-01

Silicon is an excellent material for microelectronics and integrated photonics1–3 with untapped potential for mid-IR optics4. Despite broad recognition of the importance of the third dimension5,6, current lithography methods do not allow fabrication of photonic devices and functional microelements directly inside silicon chips. Even relatively simple curved geometries cannot be realised with techniques like reactive ion etching. Embedded optical elements, like in glass7, electronic devices, and better electronic-photonic integration are lacking8. Here, we demonstrate laser-based fabrication of complex 3D structures deep inside silicon using 1 µm-sized dots and rod-like structures of adjustable length as basic building blocks. The laser-modified Si has a different optical index than unmodified parts, which enables numerous photonic devices. Optionally, these parts are chemically etched to produce desired 3D shapes. We exemplify a plethora of subsurface, i.e., “in-chip” microstructures for microfluidic cooling of chips, vias, MEMS, photovoltaic applications and photonic devices that match or surpass the corresponding state-of-the-art device performances. PMID:28983323

In-chip microstructures and photonic devices fabricated by nonlinear laser lithography deep inside silicon

NASA Astrophysics Data System (ADS)

Tokel, Onur; Turnalı, Ahmet; Makey, Ghaith; Elahi, Parviz; ćolakoǧlu, Tahir; Ergeçen, Emre; Yavuz, Ã.-zgün; Hübner, René; Zolfaghari Borra, Mona; Pavlov, Ihor; Bek, Alpan; Turan, Raşit; Kesim, Denizhan Koray; Tozburun, Serhat; Ilday, Serim; Ilday, F. Ã.-mer

2017-10-01

Silicon is an excellent material for microelectronics and integrated photonics1-3, with untapped potential for mid-infrared optics4. Despite broad recognition of the importance of the third dimension5,6, current lithography methods do not allow the fabrication of photonic devices and functional microelements directly inside silicon chips. Even relatively simple curved geometries cannot be realized with techniques like reactive ion etching. Embedded optical elements7, electronic devices and better electronic-photonic integration are lacking8. Here, we demonstrate laser-based fabrication of complex 3D structures deep inside silicon using 1-µm-sized dots and rod-like structures of adjustable length as basic building blocks. The laser-modified Si has an optical index different to that in unmodified parts, enabling the creation of numerous photonic devices. Optionally, these parts can be chemically etched to produce desired 3D shapes. We exemplify a plethora of subsurface—that is, `in-chip'—microstructures for microfluidic cooling of chips, vias, micro-electro-mechanical systems, photovoltaic applications and photonic devices that match or surpass corresponding state-of-the-art device performances.

Photo-assisted etching of silicon in chlorine- and bromine-containing plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Weiye; Sridhar, Shyam; Liu, Lei

2014-05-28

Cl{sub 2}, Br{sub 2}, HBr, Br{sub 2}/Cl{sub 2}, and HBr/Cl{sub 2} feed gases diluted in Ar (50%–50% by volume) were used to study etching of p-type Si(100) in a rf inductively coupled, Faraday-shielded plasma, with a focus on the photo-assisted etching component. Etching rates were measured as a function of ion energy. Etching at ion energies below the threshold for ion-assisted etching was observed in all cases, with Br{sub 2}/Ar and HBr/Cl{sub 2}/Ar plasmas having the lowest and highest sub-threshold etching rates, respectively. Sub-threshold etching rates scaled with the product of surface halogen coverage (measured by X-ray photoelectron spectroscopy) andmore » Ar emission intensity (7504 Å). Etching rates measured under MgF{sub 2}, quartz, and opaque windows showed that sub-threshold etching is due to photon-stimulated processes on the surface, with vacuum ultraviolet photons being much more effective than longer wavelengths. Scanning electron and atomic force microscopy revealed that photo-etched surfaces were very rough, quite likely due to the inability of the photo-assisted process to remove contaminants from the surface. Photo-assisted etching in Cl{sub 2}/Ar plasmas resulted in the formation of 4-sided pyramidal features with bases that formed an angle of 45° with respect to 〈110〉 cleavage planes, suggesting that photo-assisted etching can be sensitive to crystal orientation.« less

CoPt/TiN films nanopatterned by RF plasma etching towards dot-patterned magnetic media

NASA Astrophysics Data System (ADS)

Szívós, János; Pothorszky, Szilárd; Soltys, Jan; Serényi, Miklós; An, Hongyu; Gao, Tenghua; Deák, András; Shi, Ji; Sáfrán, György

2018-03-01

CoPt thin films as possible candidates for Bit Patterned magnetic Media (BPM) were prepared and investigated by electron microscopy techniques and magnetic measurements. The structure and morphology of the Direct Current (DC) sputtered films with N incorporation were revealed in both as-prepared and annealed state. Nanopatterning of the samples was carried out by means of Radio Frequency (RF) plasma etching through a Langmuir-Blodgett film of silica nanospheres that is a fast and high throughput technique. As a result, the samples with hexagonally arranged 100 nm size separated dots of fct-phase CoPt were obtained. The influence of the order of nanopatterning and anneling on the nanostructure formation was revealed. The magnetic properties of the nanopatterned fct CoPt films were investigated by Vibrating Sample Magnetometer (VSM) and Magnetic Force Microscopy (MFM). The results show that CoPt thin film nanopatterned by means of the RF plasma etching technique is promising candidate to a possible realization of BPM. Furthermore, this technique is versatile and suitable for scaling up to technological and industrial applications.

Etching of germanium-tin using ammonia peroxide mixture

NASA Astrophysics Data System (ADS)

Dong, Yuan; Ong, Bin Leong; Wang, Wei; Zhang, Zheng; Pan, Jisheng; Gong, Xiao; Tok, Eng-Soon; Liang, Gengchiau; Yeo, Yee-Chia

2015-12-01

The wet etching of germanium-tin (Ge1-xSnx) alloys (4.2% < x < 16.0%) in ammonia peroxide mixture (APM) is investigated. Empirical fitting of the data points indicates that the etch depth of Ge1-xSnx is proportional to the square root of the etch time t and decreases exponentially with increasing x for a given t. In addition, X-ray photoelectron spectroscopy results show that increasing t increases the intensity of the Sn oxide peak, whereas no obvious change is observed for the Ge oxide peak. This indicates that an accumulation of Sn oxide on the Ge1-xSnx surface decreases the amount of Ge atoms exposed to the etchant, which accounts for the decrease in etch rate with increasing etch time. Atomic force microscopy was used to examine the surface morphologies of the Ge0.918Sn0.082 samples. Both root-mean-square roughness and undulation periods of the Ge1-xSnx surface were observed to increase with increasing t. This work provides further understanding of the wet etching of Ge1-xSnx using APM and may be used for the fabrication of Ge1-xSnx-based electronic and photonic devices.

New approaches in renal microscopy: volumetric imaging and superresolution microscopy.

PubMed

Kim, Alfred H J; Suleiman, Hani; Shaw, Andrey S

2016-05-01

Histologic and electron microscopic analysis of the kidney has provided tremendous insight into structures such as the glomerulus and nephron. Recent advances in imaging, such as deep volumetric approaches and superresolution microscopy, have the capacity to dramatically enhance our current understanding of the structure and function of the kidney. Volumetric imaging can generate images millimeters below the surface of the intact kidney. Superresolution microscopy breaks the diffraction barrier inherent in traditional light microscopy, enabling the visualization of fine structures. Here, we describe new approaches to deep volumetric and superresolution microscopy of the kidney. Rapid advances in lasers, microscopic objectives, and tissue preparation have transformed our ability to deep volumetric image the kidney. Innovations in sample preparation have allowed for superresolution imaging with electron microscopy correlation, providing unprecedented insight into the structures within the glomerulus. Technological advances in imaging have revolutionized our capacity to image both large volumes of tissue and the finest structural details of a cell. These new advances have the potential to provide additional profound observations into the normal and pathologic functions of the kidney.

Deep reactive ion etching of 4H-SiC via cyclic SF6/O2 segments

NASA Astrophysics Data System (ADS)

Luna, Lunet E.; Tadjer, Marko J.; Anderson, Travis J.; Imhoff, Eugene A.; Hobart, Karl D.; Kub, Fritz J.

2017-10-01

Cycles of inductively coupled SF6/O2 plasma with low (9%) and high (90%) oxygen content etch segments are used to produce up to 46.6 µm-deep trenches with 5.5 µm-wide openings in single-crystalline 4H-SiC substrates. The low oxygen content segment serves to etch deep in SiC whereas the high oxygen content segment serves to etch SiC at a slower rate, targeting carbon-rich residues on the surface as the combination of carbon-rich and fluorinated residues impact sidewall profile. The cycles work in concert to etch past 30 µm at an etch rate of ~0.26 µm min-1 near room temperature, while maintaining close to vertical sidewalls, high aspect ratio, and high mask selectivity. In addition, power ramps during the low oxygen content segment is used to produce a 1:1 ratio of mask opening to trench bottom width. The effect of process parameters such as cycle time and backside substrate cooling on etch depth and micromasking of the electroplated nickel etch mask are investigated.

Characterization and modeling of low energy ion-induced damage in III-V semiconductors

NASA Astrophysics Data System (ADS)

Chen, Ching-Hui

1997-11-01

Low energy ion-induced damage (sub-keV) created during dry etching processes can extend quite deeply into materials. A systematic study on the deep penetration of dry etch-induced damage is necessary to improve device performance and helpful in further understanding the nature of defect propagation in semiconductors. In this study, a phenomenological model of dry etching damage that includes both effects of ion channeling and defect diffusion has been developed. It underscores that in addition to ion channeling, enhanced defect diffusion also plays an important role in establishing the damage profile. Further, the enhanced diffusion of dry etch- induced damage was experimentally observed for the first time by investigating the influences of concurrent above- bandgap laser illumination and low energy Ar+ ion bombardment on the damage profiles of GaAs/AlGaAs and InP-GaAs/InP heterostructures. The results indicate that non-radiative recombination of electron and hole pairs at defect sites is responsible for the observed radiation enhanced diffusion. DLTS measurements are also employed to characterize the nature of the enhanced diffusion in n-GaAs and reveal that a major component of the ion- induced defects is associated with primary point defects. Using the better understanding of the damage propagation in dry etched materials, a thin layer of low temperature grown GaAs (~200A) was utilized to stop defect propagation during dry etching process. This approach has been successfully applied to reduce ion damage that would occur during the formation of a dry-etch gate recess of a high electron mobility transistor. Finally, some future experiments are proposed and conceptually described, which would further clarify some of the many outstanding issues in the understanding and mitigation of etch- induced damage.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Yang; Liu, Xiao Wei; Zhang, Hai Feng, E-mail: wy3121685@163.com

In this work, we present a method of fabricating super-hydrophobic surface on aluminum alloy substrate. The etching of aluminum surfaces has been performed using Beck's dislocation etchant for different time to create micrometer-sized irregular steps. An optimised etching time of 50 s is found to be essential before polytetrafluoroethylene (PTFE) coating, to obtain a highest water contact angle of 165±2° with a lowest contact angle hysteresis as low as 5±2°. The presence of patterned microstructure as revealed by scanning electron microscopy (SEM) together with the low surface energy ultrathin RF-sputtered PTFE films renders the aluminum alloy surfaces highly super-hydrophobic.

Effects of a pulsed Nd:YAG laser on enamel and dentin

NASA Astrophysics Data System (ADS)

Myers, Terry D.

1990-06-01

Enamel and dentin samples were exposed extraorally to a pulsed neodymium yttriuma1uminumgarnet (Nd:YAG) laser. The lased samples were observed using both scanning electron microscopy and histological techniques to determine the effects of the laser. The present study has provided the following points: (1) Properly treated, enamel can be 1aser etched to a depth comparable to that achieved with phosphoric acid etching; and (2) both carious and noncarious dentin can be vaporized by the Nd:YAG laser. No cracking or chipping of any enamel or dentin sample was observed histologically or under the SEM.

Effect of etching on bonding of a self-etch adhesive to dentine affected by amelogenesis imperfecta.

PubMed

Epasinghe, Don Jeevanie; Yiu, Cynthia Kar Yung

2018-02-01

Dentine affected by amelogenesis imperfecta (AI) is histologically altered due to loss of hypoplastic enamel and becomes hypermineralized. In the present study, we examined the effect of additional acid etching on microtensile bond strength of a self-etch adhesive to AI-affected dentine. Flat coronal dentine obtained from extracted AI-affected and non-carious permanent molars were allocated to two groups: (a) Clearfil SE Bond (control); and (b) Clearfil SE Bond and additional etching with 34% phosphoric acid for 15 seconds. The bonded teeth were sectioned into .8-mm 2 beams for microtensile bond strength testing, and stressed to failure under tension. The bond strength data were analyzed using two-way analysis of variance (dentine type and etching step) and Student-Newman-Keuls multiple comparison test (P<.05). Representative fractured beams from each group were examined under scanning electron microscopy. Both factors, dentine substrate (P<.001) and etching step (P<.05), and their interactions (P<.001), were statistically significant. Additional etching had an adverse effect on the bond strength of Clearfil SE Bond to normal dentine (P<.005), and no significant improvement was found for AI-affected dentine (P=.479). Additional acid etching does not improve the bond strength of a self-etch adhesive to AI-affected dentine. © 2017 John Wiley & Sons Australia, Ltd.

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

Fundamental technical elements of freeze-fracture/freeze-etch in biological electron microscopy.

PubMed

Carson, Johnny L

2014-09-11

Freeze-fracture/freeze-etch describes a process whereby specimens, typically biological or nanomaterial in nature, are frozen, fractured, and replicated to generate a carbon/platinum "cast" intended for examination by transmission electron microscopy. Specimens are subjected to ultrarapid freezing rates, often in the presence of cryoprotective agents to limit ice crystal formation, with subsequent fracturing of the specimen at liquid nitrogen cooled temperatures under high vacuum. The resultant fractured surface is replicated and stabilized by evaporation of carbon and platinum from an angle that confers surface three-dimensional detail to the cast. This technique has proved particularly enlightening for the investigation of cell membranes and their specializations and has contributed considerably to the understanding of cellular form to related cell function. In this report, we survey the instrument requirements and technical protocol for performing freeze-fracture, the associated nomenclature and characteristics of fracture planes, variations on the conventional procedure, and criteria for interpretation of freeze-fracture images. This technique has been widely used for ultrastructural investigation in many areas of cell biology and holds promise as an emerging imaging technique for molecular, nanotechnology, and materials science studies.

Self-Healing Thermal Annealing: Surface Morphological Restructuring Control of GaN Nanorods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Conroy, Michele; Li, Haoning; Zubialevich, Vitaly Z.

With advances in nanolithography and dry etching, top-down methods of nanostructuring have become a widely used tool for improving the efficiency of optoelectronics. These nano dimensions can offer various benefits to the device performance in terms of light extraction and efficiency, but often at the expense of emission color quality. Broadening of the target emission peak and unwanted yellow luminescence are characteristic defect-related effects due to the ion beam etching damage, particularly for III–N based materials. In this article we focus on GaN based nanorods, showing that through thermal annealing the surface roughness and deformities of the crystal structure canmore » be “self-healed”. Correlative electron microscopy and atomic force microscopy show the change from spherical nanorods to faceted hexagonal structures, revealing the temperature-dependent surface morphology faceting evolution. The faceted nanorods were shown to be strain- and defect-free by cathodoluminescence hyperspectral imaging, micro-Raman, and transmission electron microscopy (TEM). In-situ TEM thermal annealing experiments allowed for real time observation of dislocation movements and surface restructuring observed in ex-situ annealing TEM sampling. This thermal annealing investigation gives new insight into the redistribution path of GaN material and dislocation movement post growth, allowing for improved understanding and in turn advances in optoelectronic device processing of compound semiconductors.« less

Wavelength Independent Optical Microscopy and Lithography

DTIC Science & Technology

1987-10-31

methods have been used in the past to fabricate the submicron apertures needed in near-field microscopy (2-4). However, under this contract we developed an...screens. Durig, et al. (4) in Zurich produced apertures at the tip of a single crystal of quartz etched using HF to make a fine point and covered...stage pulling process was used . Scanning electron li __ NO iI |06 j JlliM ° wm ..... 3 micrographs of a 100nm diameter pipette and a 500nm diameter

Alternating SiCl4/O2 passivation steps with SF6 etch steps for silicon deep etching

NASA Astrophysics Data System (ADS)

Duluard, C. Y.; Ranson, P.; Pichon, L. E.; Pereira, J.; Oubensaid, E. H.; Lefaucheux, P.; Puech, M.; Dussart, R.

2011-06-01

Deep etching of silicon has been investigated in an inductively coupled plasma etch reactor using short SiCl4/O2 plasma steps to passivate the sidewalls of the etched structures. A study was first carried out to define the appropriate parameters to create, at a substrate temperature of -20 °C, a passivation layer by SiCl4/O2 plasma that resists lateral chemical etching in SF6 plasma. The most efficient passivation layer was obtained for a SiCl4/O2 gas flow ratio of 2:1, a pressure of 1 Pa and a source power of 1000 W. Ex situ analyses on a film deposited with these parameters show that it is very rich in oxygen. Silicon etching processes that alternate SF6 plasma etch steps with SiCl4/O2 plasma passivation steps were then developed. Preliminary tests in pulsed-mode conditions have enabled etch rates greater than 2 µm min-1 with selectivities higher than 220. These results show that it is possible to develop a silicon deep etching process at substrate temperatures around -20 °C that uses low SiCl4 and O2 gas flows instead of conventional fluorocarbon gases for sidewall protection.

Evaluation of biofouling in stainless microfluidic channels for implantable multilayered dialysis device

NASA Astrophysics Data System (ADS)

Ota, Takashi; To, Naoya; Kanno, Yoshihiko; Miki, Norihisa

2017-06-01

An implantable artificial kidney can markedly improve the quality of life of renal disease patients. Our group has developed an implantable multilayered dialysis system consisting of microfluidic channels and dialysis membranes. Long-term evaluation is necessary for implant devices where biofouling is a critical factor, culminating in the deterioration of dialysis performance. Our previous work revealed that surface conditions, which depend on the manufacturing process, determine the amount of biofouling, and that electrolytic etching is the most suitable technique for forming a channel wall free of biofouling. In this study, we investigated the electrolytic etching conditions in detail. We conducted in vitro experiments for 7 d and evaluated the adhesion of biomaterials by scanning electron microscopy. The experiments revealed that a surface mirror-finished by electrolytic etching effectively prevents biofouling.

The Effect of Phosphoric Acid Pre-etching Times on Bonding Performance and Surface Free Energy with Single-step Self-etch Adhesives.

PubMed

Tsujimoto, A; Barkmeier, W W; Takamizawa, T; Latta, M A; Miyazaki, M

2016-01-01

The purpose of this study was to evaluate the effect of phosphoric acid pre-etching times on shear bond strength (SBS) and surface free energy (SFE) with single-step self-etch adhesives. The three single-step self-etch adhesives used were: 1) Scotchbond Universal Adhesive (3M ESPE), 2) Clearfil tri-S Bond (Kuraray Noritake Dental), and 3) G-Bond Plus (GC). Two no pre-etching groups, 1) untreated enamel and 2) enamel surfaces after ultrasonic cleaning with distilled water for 30 seconds to remove the smear layer, were prepared. There were four pre-etching groups: 1) enamel surfaces were pre-etched with phosphoric acid (Etchant, 3M ESPE) for 3 seconds, 2) enamel surfaces were pre-etched for 5 seconds, 3) enamel surfaces were pre-etched for 10 seconds, and 4) enamel surfaces were pre-etched for 15 seconds. Resin composite was bonded to the treated enamel surface to determine SBS. The SFEs of treated enamel surfaces were determined by measuring the contact angles of three test liquids. Scanning electron microscopy was used to examine the enamel surfaces and enamel-adhesive interface. The specimens with phosphoric acid pre-etching showed significantly higher SBS and SFEs than the specimens without phosphoric acid pre-etching regardless of the adhesive system used. SBS and SFEs did not increase for phosphoric acid pre-etching times over 3 seconds. There were no significant differences in SBS and SFEs between the specimens with and without a smear layer. The data suggest that phosphoric acid pre-etching of ground enamel improves the bonding performance of single-step self-etch adhesives, but these bonding properties do not increase for phosphoric acid pre-etching times over 3 seconds.

Preparation of Chemically Etched Tips for Ambient Instructional Scanning Tunneling Microscopy

ERIC Educational Resources Information Center

Zaccardi, Margot J.; Winkelmann, Kurt; Olson, Joel A.

2010-01-01

A first-year laboratory experiment that utilizes concepts of electrochemical tip etching for scanning tunneling microscopy (STM) is described. This experiment can be used in conjunction with any STM experiment. Students electrochemically etch gold STM tips using a time-efficient method, which can then be used in an instructional grade STM that…

Tuning micropillar tapering for optimal friction performance of thermoplastic gecko-inspired adhesive.

PubMed

Kim, Yongkwan; Chung, Yunsie; Tsao, Angela; Maboudian, Roya

2014-05-14

We present a fabrication method and friction testing of a gecko-inspired thermoplastic micropillar array with control over the tapering angle of the pillar sidewall. A combination of deep reactive ion etching of vertical silicon pillars and subsequent maskless chemical etching produces templates with various widths and degrees of taper, which are then replicated with low-density polyethylene. As the silicon pillars on the template are chemically etched in a bath consisting of hydrofluoric acid, nitric acid, and acetic acid (HNA), the pillars are progressively thinned, then shortened. The replicated polyethylene pillar arrays exhibit a corresponding increase in friction as the stiffness is reduced with thinning and then a decrease in friction as the stiffness is again increased. The dilution of the HNA bath in water influences the tapering angle of the silicon pillars. The friction of the replicated pillars is maximized for the taper angle that maximizes the contact area at the tip which in turn is influenced by the stiffness of the tapered pillars. To provide insights on how changes in microscale geometry and contact behavior may affect friction of the pillar array, the pillars are imaged by scanning electron microscopy after friction testing, and the observed deformation behavior from shearing is related to the magnitude of the macroscale friction values. It is shown that the tapering angle critically changes the pillar compliance and the available contact area. Simple finite element modeling calculations are performed to support that the observed deformation is consistent with what is expected from a mechanical analysis. We conclude that friction can be maximized via proper pillar tapering with low stiffness that still maintains enough contact area to ensure high adhesion.

Exposure Characteristics of Nanoparticles as Process By-products for the Semiconductor Manufacturing Industry.

PubMed

Choi, Kwang-Min; Kim, Jin-Ho; Park, Ju-Hyun; Kim, Kwan-Sick; Bae, Gwi-Nam

2015-01-01

This study aims to elucidate the exposure properties of nanoparticles (NPs; <100 nm in diameter) in semiconductor manufacturing processes. The measurements of airborne NPs were mainly performed around process equipment during fabrication processes and during maintenance. The number concentrations of NPs were measured using a water-based condensation particle counter having a size range of 10-3,000 nm. The chemical composition, size, and shape of NPs were determined by scanning electron microscopy and transmission electron microscopy techniques equipped with energy dispersive spectroscopy. The resulting concentrations of NPs ranged from 0.00-11.47 particles/cm(3). The concentration of NPs measured during maintenance showed a tendency to increase, albeit incrementally, compared to that measured during normal conditions (under typical process conditions without maintenance). However, the increment was small. When comparing the mean number concentration and standard deviation (n ± σ) of NPs, the chemical mechanical polishing (CMP) process was the highest (3.45 ± 3.65 particles/cm(3)), and the dry etch (ETCH) process was the lowest (0.11 ± 0.22 particles/cm(3)). The major NPs observed were silica (SiO2) and titania (TiO2) particles, which were mainly spherical agglomerates ranging in size from 25-280 nm. Sampling of semiconductor processes in CMP, chemical vapor deposition, and ETCH reveled NPs were <100 nm in those areas. On the other hand, particle size exceeded 100 nm in diffusion, metallization, ion implantation, and wet cleaning/etching process. The results show that the SiO2 and TiO2 are the major NPs present in semiconductor cleanroom environments.

Effect of postoperative peroxide bleaching on the marginal seal of composite restorations bonded with self-etch adhesives.

PubMed

Roubickova, A; Dudek, M; Comba, L; Housova, D; Bradna, P

2013-01-01

The aim of this study was to determine the effect of peroxide bleaching on the marginal seal of composite restorations bonded with several adhesive systems. Combined cylindrical Class V cavities located half in enamel and half in dentin were prepared on the buccal and lingual surfaces of human molars. The cavities were bonded with the self-etch adhesives Clearfil SE-Bond (CLF), Adper Prompt (ADP), and iBond (IBO) and an etch-and-rinse adhesive Gluma Comfort Bond (GLU) and restored with a microhybrid composite Charisma. Experimental groups were treated 25 times for eight hours per day with a peroxide bleaching gel Opalescence PF 20, while the control groups were stored in distilled water for two months and then subjected to a microleakage test using a dye penetration method. Scanning electron microscopy was used to investigate the etching and penetration abilities of the adhesives and morphology of debonded restoration-enamel interfaces after the microleakage tests. Statistical analyses were performed using nonparametric Kruskal-Wallis, Mann-Whitney, and Wilcoxon tests at p=0.05. The microleakage of all GLU groups was low and not significantly affected by peroxide bleaching. Low microleakage was recorded for CLF control groups, but after bleaching, a small but significant increase in microleakage at the enamel margin indicated its sensitivity to peroxide bleaching. For ADP and IBO control groups, the microleakage at the enamel margins was significantly higher than for GLU and CLF and exceeded that at the dentin margins. Bleaching did not induce any significant changes in the microleakage. Electron microscopy analysis indicated that in our experimental setup, decreased adhesion and mechanical resistance of the ADP- and IBO-enamel interfaces could be more important than the chemical degradation effects induced by the peroxide bleaching gel.

Titanium Surface Roughing Treatments contribute to Higher Interaction with Salivary Proteins MG2 and Lactoferrin.

PubMed

Cavalcanti, Yuri Wanderley; Soare, Rodrigo Villamarim; Leite Assis, Marina Araújo; Zenóbio, Elton Gonçalves; Girundi, Francisco Mauro da Silva

2015-02-01

Some surface treatments performed on titanium can alter the composition of salivary pellicle formed on this abiotic surface. Such treatments modify the titanium's surface properties and can promote higher adsorption of proteins, which allow better integration of titanium to the biotic system. This study aimed to evaluate the interactions between salivary proteins and titanium disks with different surface treatments. Machined titanium disks (n = 48) were divided into four experimental groups (n = 12), according to their surface treatments: surface polishing (SP); acid etching (A); spot-blasting plus acid etching (SB-A); spot-blasting followed by acid etching and nano-functionalization (SB-A-NF). Titanium surfaces were characterized by surface roughness and scanning electron microscopy (SEM). Specimens were incubated with human saliva extracted from submandibular and sublingual glands. Total salivary protein adsorbed to titanium was quantified and samples were submitted to western blotting for mucin glycoprotein 2 (MG2) and lactoferrin identification. Surface roughness was statistically higher for SB-A and SB-A-NF groups. Scanning electron microscopy images confirmed that titanium surface treatments increased surface roughness with higher number of porous and scratches for SB-A and SB-A-NF groups. Total protein adsorption was significantly higher for SB-A and SB-A-NF groups (p < 0.05), which also presented higher interactions with MG2 and lactoferrin proteins. The roughing of titanium surface by spot-blasting plus acid etching treatments contribute to higher interaction with salivary proteins, such as MG2 and lactoferrin. Titanium surface roughing increases the interactions of the substratum with salivary proteins, which can influence the integration of dental implants and their components to the oral environment. However, those treatments should be used carefully intraorally, avoiding increase biofilm formation.

Mechanical and chemical effects of ion-texturing biomedical polymers

NASA Technical Reports Server (NTRS)

Weigand, A. J.; Cenkus, M. A.

1979-01-01

To determine whether sputter etching may provide substantial polymer surface texturing with insignificant changes in chemical and mechanical properties, an 8 cm beam diameter, electron bombardment, argon ion source was used to sputter etch (ion-texture process) nine biomedical polymers. The materials included silicone rubber, 32% carbon impregnated polyolefin, polyoxymethylene, polytetrafluoroethylene, ultrahigh molecular weight (UHMW) polyethylene, UHMW polyethylene with carbon fibers (10%), and several polyurethanes (bioelectric, segmented, and cross linked). Ion textured microtensile specimens of each material except UHMW polyethylene and UHMW polyethylene with 10% carbon fibers were used to determine the effect of ion texturing on tensile properties. Scanning electron microscopy was used to determine surface morphology changes, and electron spectroscopy for chemical analysis was used to analyze the near surface chemical changes that result from ion texturing. Ion energies of 500 eV with beam current densities ranging from 0.08 to 0.19 mA/sq cm were used to ion texture the various materials. Standard microtensile specimens of seven polymers were exposed to a saline environment for 24 hours prior to and during the tensile testing. The surface chemical changes resulting from sputter etching are minimal in spite of the often significant changes in the surface morphology.

Atomic layer deposition frequency-multiplied Fresnel zone plates for hard x-rays focusing

DOE PAGES

Moldovan, Nicolaie; Divan, Ralu; Zeng, Hongjun; ...

2017-12-01

The design and fabrication of Fresnel zone plates for hard x-ray focusing up to 25 keV photon energies with better than 50 nm imaging half-pitch resolution is reported as performed by forming an ultrananocrystalline diamond (UNCD) scaffold, subsequently coating it with atomic layer deposition (ALD) with an absorber/phase shifting material, followed by back side etching of Si to form a diamond membrane device. The scaffold is formed by chemical vapor-deposited UNCD, electron beam lithography, and deep-reactive ion etching of diamond to desired specifications. The benefits of using diamond are as follows: improved mechanical robustness to prevent collapse of high-aspect-ratio ringmore » structures, a known high-aspect-ratio etch method, excellent radiation hardness, extremely low x-ray absorption, and significantly improved thermal/dimensional stability as compared to alternative materials. Central to the technology is the high-resolution patterning of diamond membranes at wafer scale, which was pushed to 60 nm lines and spaces etched 2.2-mu m-deep, to an aspect ratio of 36:1. The absorber growth was achieved by ALD of Ir, Pt, or W, while wafer-level processing allowed to obtain up to 121 device chips per 4 in. wafer with yields better than 60%. X-ray tests with such zone plates allowed resolving 50 nm lines and spaces, at the limit of the available resolution test structures.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moldovan, Nicolaie; Divan, Ralu; Zeng, Hongjun

The design and fabrication of Fresnel zone plates for hard x-ray focusing up to 25 keV photon energies with better than 50 nm imaging half-pitch resolution is reported as performed by forming an ultrananocrystalline diamond (UNCD) scaffold, subsequently coating it with atomic layer deposition (ALD) with an absorber/phase shifting material, followed by back side etching of Si to form a diamond membrane device. The scaffold is formed by chemical vapor-deposited UNCD, electron beam lithography, and deep-reactive ion etching of diamond to desired specifications. The benefits of using diamond are as follows: improved mechanical robustness to prevent collapse of high-aspect-ratio ringmore » structures, a known high-aspect-ratio etch method, excellent radiation hardness, extremely low x-ray absorption, and significantly improved thermal/dimensional stability as compared to alternative materials. Central to the technology is the high-resolution patterning of diamond membranes at wafer scale, which was pushed to 60 nm lines and spaces etched 2.2-mu m-deep, to an aspect ratio of 36:1. The absorber growth was achieved by ALD of Ir, Pt, or W, while wafer-level processing allowed to obtain up to 121 device chips per 4 in. wafer with yields better than 60%. X-ray tests with such zone plates allowed resolving 50 nm lines and spaces, at the limit of the available resolution test structures.« less

Vertically aligned nanowires from boron-doped diamond.

PubMed

Yang, Nianjun; Uetsuka, Hiroshi; Osawa, Eiji; Nebel, Christoph E

2008-11-01

Vertically aligned diamond nanowires with controlled geometrical properties like length and distance between wires were fabricated by use of nanodiamond particles as a hard mask and by use of reactive ion etching. The surface structure, electronic properties, and electrochemical functionalization of diamond nanowires were characterized by atomic force microscopy (AFM) and scanning tunneling microscopy (STM) as well as electrochemical techniques. AFM and STM experiments show that diamond nanowire etched for 10 s have wire-typed structures with 3-10 nm in length and with typically 11 nm spacing in between. The electrode active area of diamond nanowires is enhanced by a factor of 2. The functionalization of nanowire tips with nitrophenyl molecules is characterized by STM on clean and on nitrophenyl molecule-modified diamond nanowires. Tip-modified diamond nanowires are promising with respect to biosensor applications where controlled biomolecule bonding is required to improve chemical stability and sensing significantly.

Shape transition in nano-pits after solid-phase etching of SiO{sub 2} by Si islands

DOE Office of Scientific and Technical Information (OSTI.GOV)

Leroy, F.; Curiotto, S.; Cheynis, F.

2015-05-11

We study the nano-pits formed during the etching of a SiO{sub 2} film by reactive Si islands at T≈1000 °C. Combining low energy electron microscopy, atomic force microscopy, kinetic Monte Carlo simulations, and an analytic model based on reaction and diffusion at the solid interface, we show that the shape of the nanopits depend on the ratio R/x{sub s} with R the Si island radius and x{sub s} the oxygen diffusion-length at the Si/SiO{sub 2} interface. For small R/x{sub s}, nanopits exhibit a single-well V-shape, while a double-well W-shape is found for larger R/x{sub s}. The analysis of the transition revealsmore » that x{sub s}∼60 nm at T≈1000 °C.« less

Suppression of Lateral Diffusion and Surface Leakage Currents in nBn Photodetectors Using an Inverted Design

NASA Astrophysics Data System (ADS)

Du, X.; Savich, G. R.; Marozas, B. T.; Wicks, G. W.

2018-02-01

Surface leakage and lateral diffusion currents in InAs-based nBn photodetectors have been investigated. Devices fabricated using a shallow etch processing scheme that etches through the top contact and stops at the barrier exhibited large lateral diffusion current but undetectably low surface leakage. Such large lateral diffusion current significantly increased the dark current, especially in small devices, and causes pixel-to-pixel crosstalk in detector arrays. To eliminate the lateral diffusion current, two different approaches were examined. The conventional solution utilized a deep etch process, which etches through the top contact, barrier, and absorber. This deep etch processing scheme eliminated lateral diffusion, but introduced high surface current along the device mesa sidewalls, increasing the dark current. High device failure rate was also observed in deep-etched nBn structures. An alternative approach to limit lateral diffusion used an inverted nBn structure that has its absorber grown above the barrier. Like the shallow etch process on conventional nBn structures, the inverted nBn devices were fabricated with a processing scheme that only etches the top layer (the absorber, in this case) but avoids etching through the barrier. The results show that inverted nBn devices have the advantage of eliminating the lateral diffusion current without introducing elevated surface current.

Bio-inspired silicon nanospikes fabricated by metal-assisted chemical etching for antibacterial surfaces

NASA Astrophysics Data System (ADS)

Hu, Huan; Siu, Vince S.; Gifford, Stacey M.; Kim, Sungcheol; Lu, Minhua; Meyer, Pablo; Stolovitzky, Gustavo A.

2017-12-01

The recently discovered bactericidal properties of nanostructures on wings of insects such as cicadas and dragonflies have inspired the development of similar nanostructured surfaces for antibacterial applications. Since most antibacterial applications require nanostructures covering a considerable amount of area, a practical fabrication method needs to be cost-effective and scalable. However, most reported nanofabrication methods require either expensive equipment or a high temperature process, limiting cost efficiency and scalability. Here, we report a simple, fast, low-cost, and scalable antibacterial surface nanofabrication methodology. Our method is based on metal-assisted chemical etching that only requires etching a single crystal silicon substrate in a mixture of silver nitrate and hydrofluoric acid for several minutes. We experimentally studied the effects of etching time on the morphology of the silicon nanospikes and the bactericidal properties of the resulting surface. We discovered that 6 minutes of etching results in a surface containing silicon nanospikes with optimal geometry. The bactericidal properties of the silicon nanospikes were supported by bacterial plating results, fluorescence images, and scanning electron microscopy images.

Maskless and low-destructive nanofabrication on quartz by friction-induced selective etching

PubMed Central

2013-01-01

A low-destructive friction-induced nanofabrication method is proposed to produce three-dimensional nanostructures on a quartz surface. Without any template, nanofabrication can be achieved by low-destructive scanning on a target area and post-etching in a KOH solution. Various nanostructures, such as slopes, hierarchical stages and chessboard-like patterns, can be fabricated on the quartz surface. Although the rise of etching temperature can improve fabrication efficiency, fabrication depth is dependent only upon contact pressure and scanning cycles. With the increase of contact pressure during scanning, selective etching thickness of the scanned area increases from 0 to 2.9 nm before the yield of the quartz surface and then tends to stabilise after the appearance of a wear. Refabrication on existing nanostructures can be realised to produce deeper structures on the quartz surface. Based on Arrhenius fitting of the etching rate and transmission electron microscopy characterization of the nanostructure, fabrication mechanism could be attributed to the selective etching of the friction-induced amorphous layer on the quartz surface. As a maskless and low-destructive technique, the proposed friction-induced method will open up new possibilities for further nanofabrication. PMID:23531381

Si substrates texturing and vapor-solid-solid Si nanowhiskers growth using pure hydrogen as source gas

NASA Astrophysics Data System (ADS)

Nordmark, H.; Nagayoshi, H.; Matsumoto, N.; Nishimura, S.; Terashima, K.; Marioara, C. D.; Walmsley, J. C.; Holmestad, R.; Ulyashin, A.

2009-02-01

Scanning and transmission electron microscopies have been used to study silicon substrate texturing and whisker growth on Si substrates using pure hydrogen source gas in a tungsten hot filament reactor. Substrate texturing, in the nanometer to micrometer range of mono- and as-cut multicrystalline silicon, was observed after deposition of WSi2 particles that acted as a mask for subsequent hydrogen radical etching. Simultaneous Si whisker growth was observed for long residence time of the source gas and low H2 flow rate with high pressure. The whiskers formed via vapor-solid-solid growth, in which the deposited WSi2 particles acted as catalysts for a subsequent metal-induced layer exchange process well below the eutectic temperature. In this process, SiHx species, formed by substrate etching by the H radicals, diffuse through the metal particles. This leads to growth of crystalline Si whiskers via metal-induced solid-phase crystallization. Transmission electron microscopy, electron diffraction, and x-ray energy dispersive spectroscopy were used to study the WSi2 particles and the structure of the Si substrates in detail. It has been established that the whiskers are partly crystalline and partly amorphous, consisting of pure Si with WSi2 particles on their tips as well as sometimes being incorporated into their structure.

Effects of hard mask etch on final topography of advanced phase shift masks

NASA Astrophysics Data System (ADS)

Hortenbach, Olga; Rolff, Haiko; Lajn, Alexander; Baessler, Martin

2017-07-01

Continuous shrinking of the semiconductor device dimensions demands steady improvements of the lithographic resolution on wafer level. These requirements challenge the photomask industry to further improve the mask quality in all relevant printing characteristics. In this paper topography of the Phase Shift Masks (PSM) was investigated. Effects of hard mask etch on phase shift uniformity and mask absorber profile were studied. Design of experiments method (DoE) was used for the process optimization, whereas gas composition, bias power of the hard mask main etch and bias power of the over-etch were varied. In addition, influence of the over-etch time was examined at the end of the experiment. Absorber depth uniformity, sidewall angle (SWA), reactive ion etch lag (RIE lag) and through pitch (TP) dependence were analyzed. Measurements were performed by means of Atomic-force microscopy (AFM) using critical dimension (CD) mode with a boot-shaped tip. Scanning electron microscope (SEM) cross-section images were prepared to verify the profile quality. Finally CD analysis was performed to confirm the optimal etch conditions. Significant dependence of the absorber SWA on hard mask (HM) etch conditions was observed revealing an improvement potential for the mask absorber profile. It was found that hard mask etch can leave a depth footprint in the absorber layer. Thus, the etch depth uniformity of hard mask etch is crucial for achieving a uniform phase shift over the active mask area. The optimized hard mask etch process results in significantly improved mask topography without deterioration of tight CD specifications.

Surface modification with alumina blasting and H2SO4-HCl etching for bonding two resin-composite veneers to titanium.

PubMed

Taira, Yohsuke; Egoshi, Takafumi; Kamada, Kohji; Sawase, Takashi

2014-02-01

The purpose of this study was to investigate the effect of an experimental surface treatment with alumina blasting and acid etching on the bond strengths between each of two resin composites and commercially pure titanium. The titanium surface was blasted with alumina and then etched with 45wt% H2SO4 and 15wt% HCl (H2SO4-HCl). A light- and heat-curing resin composite (Estenia) and a light-curing resin composite (Ceramage) were used with adjunctive metal primers. Veneered specimens were subjected to thermal cycling between 4 and 60°C for 50,000 cycles, and the shear bond strengths were determined. The highest bond strengths were obtained for Blasting/H2SO4-HCl/Estenia (30.2 ± 4.5 MPa) and Blasting/Etching/Ceramage (26.0 ± 4.5 MPa), the values of which were not statistically different, followed by Blasting/No etching/Estenia (20.4 ± 2.4 MPa) and Blasting/No etching/Ceramage (0.8 ± 0.3 MPa). Scanning electron microscopy observations revealed that alumina blasting and H2SO4-HCl etching creates a number of micro- and nanoscale cavities on the titanium surface, which contribute to adhesive bonding. © 2013 Eur J Oral Sci.

Influence of the doping type and level on the morphology of porous Si formed by galvanic etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pyatilova, O. V., E-mail: 5ilova87@gmail.com; Gavrilov, S. A.; Shilyaeva, Yu. I.

The formation of porous silicon (por-Si) layers by the galvanic etching of single-crystal Si samples (doped with boron or phosphorus) in an HF/C{sub 2}H{sub 5}OH/H{sub 2}O{sub 2} solution is investigated. The por-Si layers are analyzed by the capillary condensation of nitrogen and scanning electron microscopy (SEM). The dependences of the morphological characteristics of por-Si (pore diameter, specific surface area, pore volume, and thickness of the pore walls), which determine the por-Si combustion kinetics, on the dopant type and initial wafer resistivity are established.

Refractive index profiles of Ge-doped optical fibers with nanometer spatial resolution using atomic force microscopy.

PubMed

Pace, P; Huntington, Shane; Lyytikäinen, K; Roberts, A; Love, J

2004-04-05

We show a quantitative connection between Refractive Index Profiles (RIP) and measurements made by an Atomic Force Microscope (AFM). Germanium doped fibers were chemically etched in hydrofluoric acid solution (HF) and the wet etching characteristics of germanium were studied using an AFM. The AFM profiles were compared to both a concentration profile of the preform determined using a Scanning Electron Microscope (SEM) and a RIP of the fiber measured using a commercial profiling instrument, and were found to be in excellent agreement. It is now possible to calculate the RIP of a germanium doped fiber directly from an AFM profile.

Spectroscopic and microscopic investigation of MBE-grown CdTe (211)B epitaxial thin films on GaAs (211)B substrates

NASA Astrophysics Data System (ADS)

Özden, Selin; Koc, Mumin Mehmet

2018-03-01

CdTe epitaxial thin films, for use as a buffer layer for HgCdTe defectors, were grown on GaAs (211)B using the molecular beam epitaxy method. Wet chemical etching (Everson method) was applied to the epitaxial films using various concentrations and application times to quantify the crystal quality and dislocation density. Surface characterization of the epitaxial films was achieved using Atomic force microscopy and Scanning electron microscopy (SEM) before and after each treatment. The Energy Dispersive X-Ray apparatus of SEM was used to characterize the chemical composition. Untreated CdTe films show smooth surface characteristics with root mean square (RMS) roughnesses of 1.18-3.89 nm. The thicknesses of the CdTe layers formed were calculated via FTIR spectrometry and obtained by ex situ spectroscopic ellipsometry. Raman spectra were obtained for various temperatures. Etch pit densities (EPD) were measured, from which it could be seen that EPD changes between 1.7 × 108 and 9.2 × 108 cm-2 depending on the concentration of the Everson etch solution and treatment time. Structure, shape and depth of pits resulting from each etch pit implementation were also evaluated. Pit widths varying between 0.15 and 0.71 µm with heights varying between 2 and 80 nm were observed. RMS roughness was found to vary by anything from 1.56 to 26 nm.

Homogeneous alignment of nematic liquid crystals by ion beam etched surfaces

NASA Technical Reports Server (NTRS)

Wintucky, E. G.; Mahmood, R.; Johnson, D. L.

1979-01-01

A wide range of ion beam etch parameters capable of producing uniform homogeneous alignment of nematic liquid crystals on SiO2 films are discussed. The alignment surfaces were generated by obliquely incident (angles of 5 to 25 deg) argon ions with energies in the range of 0.5 to 2.0 KeV, ion current densities of 0.1 to 0.6 mA sq cm and etch times of 1 to 9 min. A smaller range of ion beam parameters (2.0 KeV, 0.2 mA sq cm, 5 to 10 deg and 1 to 5 min.) were also investigated with ZrO2 films and found suitable for homogeneous alignment. Extinction ratios were very high (1000), twist angles were small ( or = 3 deg) and tilt-bias angles very small ( or = 1 deg). Preliminary scanning electron microscopy results indicate a parallel oriented surface structure on the ion beam etched surfaces which may determine alignment.

Photoluminescence of etched SiC nanowires

NASA Astrophysics Data System (ADS)

Stewart, Polite D., Jr.; Rich, Ryan; Zerda, T. W.

2010-10-01

SiC nanowires were produced from carbon nanotubes and nanosize silicon powder in a tube furnace at temperatures between 1100^oC and 1350^oC. SiC nanowires had average diameter of 30 nm and very narrow size distribution. The compound possesses a high melting point, high thermal conductivity, and excellent wear resistance. The surface of the SiC nanowires after formation is covered by an amorphous layer. The composition of that layer is not fully understood, but it is believed that in addition to amorphous SiC it contains various carbon and silicon compounds, and SiO2. The objective of the research was to modify the surface structure of these SiC nanowires. Modification of the surface was done using the wet etching method. The etched nanowires were then analyzed using Fourier Transform Infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and photoluminescence (PL). FTIR and TEM analysis provided valid proof that the SiC nanowires were successfully etched. Also, the PL results showed that the SiC nanowire core did possess a fluorescent signal.

The influence of H{sub 2}O{sub 2} concentration to the structure of silicon nanowire growth by metal-assisted chemical etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Omar, Hafsa, E-mail: mrshafsaomar@gmail.com; Jani, Abdul Mutalib Md., E-mail: abdmutalib@perlis.uitm.edu.my; Abdullah, Saifollah, E-mail: saifollah@salam.utm.edu.my

2016-07-06

A simple and low cost method to produce well aligned silicon nanowires at large areas using Ag-assisted chemical etching at room temperature were presented. The structure of silicon nanowires growth by metal-assisted chemical etching was observed. Prior to the etching, the silicon nanowires were prepared by electroless metal deposited (EMD) in solution containing hydrofluoric acid and hydrogen peroxide in Teflon vessel. The silver particle was deposited on substrate by immersion in hydrofluoric acid and silver nitrate solution for sixty second. The silicon nanowires were growth in different hydrogen peroxide concentration which are 0.3M, 0.4M, 0.5M and 0.6M and 0.7M.The influencemore » of hydrogen peroxide concentration to the formation of silicon nanowires was studied. The morphological properties of silicon nanowires were investigated using field emission scanning electron microscopy (FESEM) and Energy Dispersive X-Ray Spectroscopy (EDS).« less

Anisotropic etching of platinum electrodes at the onset of cathodic corrosion

PubMed Central

Hersbach, Thomas J. P.; Yanson, Alexei I.; Koper, Marc T. M.

2016-01-01

Cathodic corrosion is a process that etches metal electrodes under cathodic polarization. This process is presumed to occur through anionic metallic reaction intermediates, but the exact nature of these intermediates and the onset potential of their formation is unknown. Here we determine the onset potential of cathodic corrosion on platinum electrodes. Electrodes are characterized electrochemically before and after cathodic polarization in 10 M sodium hydroxide, revealing that changes in the electrode surface start at an electrode potential of −1.3 V versus the normal hydrogen electrode. The value of this onset potential rules out previous hypotheses regarding the nature of cathodic corrosion. Scanning electron microscopy shows the formation of well-defined etch pits with a specific orientation, which match the voltammetric data and indicate a remarkable anisotropy in the cathodic etching process, favouring the creation of (100) sites. Such anisotropy is hypothesized to be due to surface charge-induced adsorption of electrolyte cations. PMID:27554398

Nanofabrication of insulated scanning probes for electromechanical imaging in liquid solutions

PubMed Central

Noh, Joo Hyon; Nikiforov, Maxim; Kalinin, Sergei V.; Vertegel, Alexey A.; Rack, Philip D.

2011-01-01

In this paper, the fabrication and electrical and electromechanical characterization of insulated scanning probes have been demonstrated in liquid solutions. The silicon cantilevers were sequentially coated with chromium and silicon dioxide, and the silicon dioxide was selectively etched at tip apex using focused electron beam induced etching (FEBIE) with XeF2 The chromium layer acted not only as the conductive path from the tip, but also as an etch resistant layer. This insulated scanning probe fabrication process is compatible with any commercial AFM tip and can be used to easily tailor the scanning probe tip properties because FEBIE does not require lithography. The suitability of the fabricated probes is demonstrated by imaging of standard topographical calibration grid as well as piezoresponse force microscopy (PFM) and electrical measurements in ambient and liquid environments. PMID:20702930

Effect of Interfacial characteristics of metal clad polymeric substrates on electrical high frequency interconnection performance

NASA Technical Reports Server (NTRS)

Bhasin, K. B.; Romanofsky, R. R.; Ponchak, G. E.; Liu, D. C.

1984-01-01

Etched metallic conductor lines on metal clad polymeric substrates are used for electronic component interconnections. Significant signal losses are observed for microstrip conductor lines used for interconnecting high frequency devices. At these frequencies, the electronic signal travels closer to the metal-polymer interface due to the skin effect. Copper-teflon interfaces were characterized by scanning electron microscopy (SEM) and Auger electron spectroscopy (AES) to determine the interfacial properties. Data relating roughness of the copper film to signal losses was compared to theory. Films used to enhance adhesion are found, to contribute to these losses.

Correlation between surface properties and wettability of multi-scale structured biocompatible surfaces

NASA Astrophysics Data System (ADS)

Gorodzha, S. N.; Surmeneva, M. A.; Prymak, O.; Wittmar, A.; Ulbricht, M.; Epple, M.; Teresov, A.; Koval, N.; Surmenev, R. A.

2015-11-01

The influence of surface properties of radio-frequency (RF) magnetron deposited hydroxyapatite (HA) and Si-containing HA coatings on wettability was studied. The composition and morphology of the coatings fabricated on titanium (Ti) were characterized using atomic force microscopy (AFM) and X-ray diffraction (XRD). The surface wettability was studied using contact angle analysis. Different geometric parameters of acid-etched (AE) and pulse electron beam (PEB)-treated Ti substrates and silicate content in the HA films resulted in the different morphology of the coatings at micro- and nano- length scales. Water contact angles for the HA coated Ti samples were evaluated as a combined effect of micro roughness of the substrate and nano-roughness of the HA films resulting in higher water contact angles compared with acid-etched (AE) or pulse electron beam (PEB) treated Ti substrates.

Morphological and chemical characterization of the dentin/resin cement interface produced with a self-etching primer.

PubMed

Walker, Mary P; Wang, Yong; Spencer, Paulette

2002-01-01

The purpose of this study was to analyze a resin cement/dentin interface by comparing the diffusion of a resin cement into dentin surfaces pretreated with a self-etching primer with or without pretreatment by conventional acid etching. Dentin surfaces of 8 unerupted human third molars were treated with a self-etch primer (Panavia 21) with or without conventional phosphoric acid pretreatment. Panavia 21 resin cement was applied according to manufacturer's instructions. Dentin/resin cement interface sections from each tooth were examined with scanning electron microscopy and micro-Raman spectroscopy. When the self-etch primer was used following conventional acid pretreatment, the resin cement did not penetrate to the depth of the zone of demineralized dentin, leaving a substantial area of exposed dentin matrix at the dentin/cement interface. In contrast, there was substantial resin cement diffusion throughout the demineralized dentin when the self-etch primer was used without acid etching pretreatment. The in vitro evaluation of resin cement penetration throughout the zone of demineralized dentin is an important step in identifying sites of exposed dentin matrix that may promote postoperative sensitivity and may leave the dentin/resin cement interface vulnerable to premature degradation under clinical conditions. In this study, the self-etch primer used alone produced substantial resin cement penetration and left no exposed dentin matrix at the dentin/resin cement interface.

Local electronic structure and photoelectrochemical activity of partial chemically etched Ti-doped hematite

NASA Astrophysics Data System (ADS)

Rioult, Maxime; Belkhou, Rachid; Magnan, Hélène; Stanescu, Dana; Stanescu, Stefan; Maccherozzi, Francesco; Rountree, Cindy; Barbier, Antoine

2015-11-01

The direct conversion of solar light into chemical energy or fuel through photoelectrochemical water splitting is promising as a clean hydrogen production solution. Ti-doped hematite (Ti:α-Fe2O3) is a potential key photoanode material, which despite its optimal band gap, excellent chemical stability, abundance, non-toxicity and low cost, still has to be improved. Here we give evidence of a drastic improvement of the water splitting performances of Ti-doped hematite photoanodes upon a HCl wet-etching. In addition to the topography investigation by atomic force microscopy, a detailed determination of the local electronic structure has been carried out in order to understand the phenomenon and to provide new insights in the understanding of solar water splitting. Using synchrotron radiation based spectromicroscopy (X-PEEM), we investigated the X-ray absorption spectral features at the L3 Fe edge of the as grown surface and of the wet-etched surface on the very same sample thanks to patterning. We show that HCl wet etching leads to substantial surface modifications of the oxide layer including increased roughness and chemical reduction (presence of Fe2 +) without changing the band gap. We demonstrate that these changes are profitable and correlated to the drastic changes of the photocatalytic activity.

Effect of the calcium silicate-based sealer removal protocols and time-point of acid etching on the dentin adhesive interface.

PubMed

Morais, Jéssika Mayhara Pereira; Victorino, Keli Regina; Escalante-Otárola, Wilfredo Gustavo; Jordão-Basso, Keren Cristina Fagundes; Palma-Dibb, Regina Guenka; Kuga, Milton Carlos

2018-06-15

The aim of the study was to evaluate the effects when acid etching on the dentin surface was immediately performed (I) or 7 days (D) after calcium silicate-based sealer (MTA Fillapex) removal, using 95% ethanol (E) or xylol (X). First study, 60 bovine incisor dentin specimens were impregnated with sealer and divided into six groups (n = 10): (EI), E + I; (XI), X + I; (ED), E + D; (XD), X + D, (UN), untreated and (MR), mechanical removal of sealer. Scanning electron microscopy (SEM) images (500×) were obtained from each specimen and scores assessed the sealer residues persistence. Second study, 60 specimens were similarly treated; however, the specimens were restored with composite resin after the removal protocols. Hybrid layer formation was evaluated using confocal laser microscopy (1,024×). Third study, 60 specimens were similarly obtained and subjected to micro-shear test to evaluate the effects of removal protocols on the bond strength of etch-and- rinse adhesive system to dentin. XI showed the highest persistence of sealer residues (p < .05), similar to MR (p > .05). EI showed the greatest hybrid layer extension, except in relation to UN (p < .05). XI and MR presented the lowest bond strength adhesive system to dentin (p < .05). Acid etching immediately after calcium silicate-based endodontic sealer removal using xylol presented the highest residues persistence and negatively affected the adhesive interface between dentin and etch-and-rinse adhesive system. © 2018 Wiley Periodicals, Inc.

Monolithically Integrated, Mechanically Resilient Carbon-Based Probes for Scanning Probe Microscopy

NASA Technical Reports Server (NTRS)

Kaul, Anupama B.; Megerian, Krikor G.; Jennings, Andrew T.; Greer, Julia R.

2010-01-01

Scanning probe microscopy (SPM) is an important tool for performing measurements at the nanoscale in imaging bacteria or proteins in biology, as well as in the electronics industry. An essential element of SPM is a sharp, stable tip that possesses a small radius of curvature to enhance spatial resolution. Existing techniques for forming such tips are not ideal. High-aspect-ratio, monolithically integrated, as-grown carbon nanofibers (CNFs) have been formed that show promise for SPM applications by overcoming the limitations present in wet chemical and separate substrate etching processes.

A new concept for spatially divided Deep Reactive Ion Etching with ALD-based passivation

NASA Astrophysics Data System (ADS)

Roozeboom, F.; Kniknie, B.; Lankhorst, A. M.; Winands, G.; Knaapen, R.; Smets, M.; Poodt, P.; Dingemans, G.; Keuning, W.; Kessels, W. M. M.

2012-12-01

Conventional Deep Reactive Ion Etching (DRIE) is a plasma etch process with alternating half-cycles of 1) Si-etching with SF6 to form gaseous SiFx etch products, and 2) passivation with C4F8 that polymerizes as a protecting fluorocarbon deposit on the sidewalls and bottom of the etched features. In this work we report on a novel alternative and disruptive technology concept of Spatially-divided Deep Reactive Ion Etching, S-DRIE, where the process is converted from the time-divided into the spatially divided regime. The spatial division can be accomplished by inert gas bearing 'curtains' of heights down to ~20 μm. These curtains confine the reactive gases to individual (often linear) injection slots constructed in a gas injector head. By horizontally moving the substrate back and forth under the head one can realize the alternate exposures to the overall cycle. A second improvement in the spatially divided approach is the replacement of the CVD-based C4F8 passivation steps by ALD-based oxide (e.g. SiO2) deposition cycles. The method can have industrial potential in cost-effective creation of advanced 3D interconnects (TSVs), MEMS manufacturing and advanced patterning, e.g., in nanoscale transistor line edge roughness using Atomic Layer Etching.

Sealing effectiveness of fissure sealant bonded with universal adhesive systems on saliva-contaminated and noncontaminated enamel

PubMed Central

Shafiei, Fereshteh; Zarean, Mehran; Razmjoei, Faranak

2018-01-01

Background The effectiveness of sealants is dependent upon their adhesion to enamel surface. The aim of the study was to evaluate the sealing ability of a pit and fissure sealant used with a universal adhesive (etch-and-rinse vs. self-etch modes) when the site is contaminated with saliva. Adhesive properties were evaluated as microleakage and scanning electron microscopic (SEM) characteristics. Material and Methods A total of 72 mandibular third molars were randomly divided into 6 groups (n=12). Occlusal pits and fissures were sealed with an unfilled resin fissure sealant (FS) material with or without saliva contamination. The groups included: 1) phosphoric acid etching + FS (control), 2) phosphoric acid etching + Scotchbond Universal (etch-and-rinse) + FS, 3) phosphoric acid etching + saliva + Scotchbond Universal (etch-and-rinse) + FS, 4) Scotchbond Universal (self-etching) + FS,5) Scotchbond Universal (self-etching) + saliva + FS, and 6) Scotchbond Universal (self-etching) + saliva + Scotchbond Universal + FS. After thermocycling, the teeth were placed in 0.5% fuchsin, sectioned, and evaluated by digital microscopy. Two samples from each group were also observed by SEM. The data were analyzed with Kruskal-Wallis and Mann-Whitney tests for a significance of p<0.05. Results There were significant differences among groups. Groups 1,2 and 4 showed the least microleakage, with no significant differences among groups. Saliva contamination led to increased microleakage and gap formation in SEM images in groups 3, 5 and 6. Conclusions The fissure sealing ability of the universal adhesive in etch-and-rinse or self-etch modes was similar to that of conventional acid etching. Saliva contamination had a negative effect on sealant adhesion to pretreated enamel. Key words:Pit and fissure sealant, Universal adhesive, Saliva. PMID:29670708

Sealing effectiveness of fissure sealant bonded with universal adhesive systems on saliva-contaminated and noncontaminated enamel.

PubMed

Memarpour, Mahtab; Shafiei, Fereshteh; Zarean, Mehran; Razmjoei, Faranak

2018-01-01

The effectiveness of sealants is dependent upon their adhesion to enamel surface. The aim of the study was to evaluate the sealing ability of a pit and fissure sealant used with a universal adhesive (etch-and-rinse vs. self-etch modes) when the site is contaminated with saliva. Adhesive properties were evaluated as microleakage and scanning electron microscopic (SEM) characteristics. A total of 72 mandibular third molars were randomly divided into 6 groups (n=12). Occlusal pits and fissures were sealed with an unfilled resin fissure sealant (FS) material with or without saliva contamination. The groups included: 1) phosphoric acid etching + FS (control), 2) phosphoric acid etching + Scotchbond Universal (etch-and-rinse) + FS, 3) phosphoric acid etching + saliva + Scotchbond Universal (etch-and-rinse) + FS, 4) Scotchbond Universal (self-etching) + FS,5) Scotchbond Universal (self-etching) + saliva + FS, and 6) Scotchbond Universal (self-etching) + saliva + Scotchbond Universal + FS. After thermocycling, the teeth were placed in 0.5% fuchsin, sectioned, and evaluated by digital microscopy. Two samples from each group were also observed by SEM. The data were analyzed with Kruskal-Wallis and Mann-Whitney tests for a significance of p <0.05. There were significant differences among groups. Groups 1,2 and 4 showed the least microleakage, with no significant differences among groups. Saliva contamination led to increased microleakage and gap formation in SEM images in groups 3, 5 and 6. The fissure sealing ability of the universal adhesive in etch-and-rinse or self-etch modes was similar to that of conventional acid etching. Saliva contamination had a negative effect on sealant adhesion to pretreated enamel. Key words: Pit and fissure sealant, Universal adhesive, Saliva.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lii-Rosales, Ann; Zhou, Yinghui; Wallingford, Mark

When using scanning tunneling microscopy, we characterize a surface carbide that forms such that Dy is deposited on the basal plane of graphite. In order to form carbide islands on terraces, Dy is first deposited at 650–800 K, which forms large metallic islands. Upon annealing at 1000 K, these clusters convert to carbide. Deposition directly at 1000 K is ineffective because nucleation on terraces is inhibited. Reaction is signaled by the fact that each carbide cluster is partially or totally surrounded by an etch pit. The etch pit is one carbon layer deep for most carbide clusters. Carbide clusters aremore » also identifiable by striations on their surfaces. Based on mass balance, and assuming that only the surface layer of carbon is involved in the reaction, the carbide has stoichiometry D y 2 C . This is Dy-rich compared with the most common bulk carbide Dy C 2 , which may reflect limited surface carbon transport to the carbide.« less

Patterning of light-extraction nanostructures on sapphire substrates using nanoimprint and ICP etching with different masking materials.

PubMed

Chen, Hao; Zhang, Qi; Chou, Stephen Y

2015-02-27

Sapphire nanopatterning is the key solution to GaN light emitting diode (LED) light extraction. One challenge is to etch deep nanostructures with a vertical sidewall in sapphire. Here, we report a study of the effects of two masking materials (SiO2 and Cr) and different etching recipes (the reaction gas ratio, the reaction pressure and the inductive power) in a chlorine-based (BCl3 and Cl2) inductively coupled plasma (ICP) etching of deep nanopillars in sapphire, and the etching process optimization. The masking materials were patterned by nanoimprinting. We have achieved high aspect ratio sapphire nanopillar arrays with a much steeper sidewall than the previous etching methods. We discover that the SiO2 mask has much slower erosion rate than the Cr mask under the same etching condition, leading to the deep cylinder-shaped nanopillars (122 nm diameter, 200 nm pitch, 170 nm high, flat top, and a vertical sidewall of 80° angle), rather than the pyramid-shaped shallow pillars (200 nm based diameter, 52 nm height, and 42° sidewall) resulted by using Cr mask. The processes developed are scalable to large volume LED manufacturing.

Enamel and dentin bond strengths of a new self-etch adhesive system.

PubMed

Walter, Ricardo; Swift, Edward J; Boushell, Lee W; Braswell, Krista

2011-12-01

statement of problem:  Self-etch adhesives typically are mildly acidic and therefore less effective than etch-and-rinse adhesives for bonding to enamel.   The purpose of this study was to evaluate the enamel and dentin shear bond strengths of a new two-step self-etch adhesive system, OptiBond XTR (Kerr Corporation, Orange, CA, USA).   The labial surfaces of 80 bovine teeth were ground to create flat, 600-grit enamel or dentin surfaces. Composite was bonded to enamel or dentin using the new two-step self-etch system or a three-step etch-and-rinse (OptiBond FL, Kerr), two-step self-etch (Clearfil SE Bond, Kuraray America, Houston, TX, USA), or one-step self-etch adhesive (Xeno IV, Dentsply Caulk, Milford, DE, USA). Following storage in water for 24 hours, shear bond strengths were determined using a universal testing machine. The enamel and dentin data sets were subjected to separate analysis of variance and Tukey's tests. Scanning electron microscopy was used to evaluate the effects of each system on enamel.   Mean shear bond strengths to enamel ranged from 18.1 MPa for Xeno IV to 41.0 MPa for OptiBond FL. On dentin, the means ranged from 33.3 MPa for OptiBond FL to 47.1 MPa for Clearfil SE Bond. OptiBond XTR performed as well as Clearfil SE Bond on dentin and as well as OptiBond FL on enamel. Field emission scanning electron microscope revealed that OptiBond XTR produced an enamel etch pattern that was less defined than that of OptiBond FL (37.5% phosphoric acid) but more defined than that of Clearfil SE Bond or Xeno IV.   The new two-step self-etch adhesive system formed excellent bonds to enamel and dentin in vitro. OptiBond XTR, a new two-step self-etch adhesive system, is a promising material for bonding to enamel as well as to dentin. © 2011 Wiley Periodicals, Inc.

Improvement of enamel bond strengths for conventional and resin-modified glass ionomers: acid-etching vs. conditioning*

PubMed Central

Zhang, Ling; Tang, Tian; Zhang, Zhen-liang; Liang, Bing; Wang, Xiao-miao; Fu, Bai-ping

2013-01-01

Objective: This study deals with the effect of phosphoric acid etching and conditioning on enamel micro-tensile bond strengths (μTBSs) of conventional and resin-modified glass ionomer cements (GICs/RMGICs). Methods: Forty-eight bovine incisors were prepared into rectangular blocks. Highly-polished labial enamel surfaces were either acid-etched, conditioned with liquids of cements, or not further treated (control). Subsequently, two matching pre-treated enamel surfaces were cemented together with one of four cements [two GICs: Fuji I (GC), Ketac Cem Easymix (3M ESPE); two RMGICs: Fuji Plus (GC), RelyX Luting (3M ESPE)] in preparation for μTBS tests. Pre-treated enamel surfaces and cement-enamel interfaces were analyzed by scanning electron microscopy (SEM). Results: Phosphoric acid etching significantly increased the enamel μTBS of GICs/RMGICs. Conditioning with the liquids of the cements produced significantly weaker or equivalent enamel μTBS compared to the control. Regardless of etching, RMGICs yielded stronger enamel μTBS than GICs. A visible hybrid layer was found at certain enamel-cement interfaces of the etched enamels. Conclusions: Phosphoric acid etching significantly increased the enamel μTBSs of GICs/RMGICs. Phosphoric acid etching should be recommended to etch the enamel margins before the cementation of the prostheses such as inlays and onlays, using GICs/RMGICs to improve the bond strengths. RMGICs provided stronger enamel bond strength than GICs and conditioning did not increase enamel bond strength. PMID:24190447

The endpoint detection technique for deep submicrometer plasma etching

NASA Astrophysics Data System (ADS)

Wang, Wei; Du, Zhi-yun; Zeng, Yong; Lan, Zhong-went

2009-07-01

The availability of reliable optical sensor technology provides opportunities to better characterize and control plasma etching processes in real time, they could play a important role in endpoint detection, fault diagnostics and processes feedback control and so on. The optical emission spectroscopy (OES) method becomes deficient in the case of deep submicrometer gate etching. In the newly developed high density inductively coupled plasma (HD-ICP) etching system, Interferometry endpoint (IEP) is introduced to get the EPD. The IEP fringe count algorithm is investigated to predict the end point, and then its signal is used to control etching rate and to call end point with OES signal in over etching (OE) processes step. The experiment results show that IEP together with OES provide extra process control margin for advanced device with thinner gate oxide.

Dry etched SiO2 Mask for HgCdTe Etching Process

NASA Astrophysics Data System (ADS)

Chen, Y. Y.; Ye, Z. H.; Sun, C. H.; Deng, L. G.; Zhang, S.; Xing, W.; Hu, X. N.; Ding, R. J.; He, L.

2016-09-01

A highly anisotropic etching process with low etch-induced damage is indispensable for advanced HgCdTe (MCT) infrared focal plane array (IRFPA) detectors. The inductively coupled plasma (ICP) enhanced reactive ion etching technique has been widely adopted in manufacturing HgCdTe IRFPA devices. An accurately patterned mask with sharp edges is decisive to accomplish pattern duplication. It has been reported by our group that the SiO2 mask functions well in etching HgCdTe with high selectivity. However, the wet process in defining the SiO2 mask is limited by ambiguous edges and nonuniform patterns. In this report, we patterned SiO2 with a mature ICP etching technique, prior to which a thin ZnS film was deposited by thermal evaporation. The SiO2 film etching can be terminated at the auto-stopping point of the ZnS layer thanks to the high selectivity of SiO2/ZnS in SF6 based etchant. Consequently, MCT etching was directly performed without any other treatment. This mask showed acceptable profile due to the maturity of the SiO2 etching process. The well-defined SiO2 pattern and the etched smooth surfaces were investigated with scanning electron microscopy and atomic force microscope. This new mask process could transfer the patterns exactly with very small etch-bias. A cavity with aspect-ratio (AR) of 1.2 and root mean square roughness of 1.77 nm was achieved first, slightly higher AR of 1.67 was also get with better mask profile. This masking process ensures good uniformity and surely benefits the delineation of shrinking pixels with its high resolution.

Real-time observation of morphological transformations in II-VI semiconducting nanobelts via environmental transmission electron microscopy

DOE PAGES

Agarwal, Rahul; Zakharov, Dmitri N.; Krook, Nadia M.; ...

2015-05-01

It has been observed that wurtzite II–VI semiconducting nanobelts transform into single-crystal, periodically branched nanostructures upon heating. The mechanism of this novel transformation has been elucidated by heating II–VI nanobelts in an environmental transmission electron microscope (ETEM) in oxidizing, reducing and inert atmospheres while observing their structural changes with high spatial resolution. The interplay of surface reconstruction of high-energy surfaces of the wurtzite phase and environment-dependent anisotropic chemical etching of certain crystal surfaces in the branching mechanism of nanobelts has been observed. Understanding of structural and chemical transformations of materials via in situ microscopy techniques and their role in designingmore » new nanostructured materials is discussed.« less

Comparison of tensile bond strengths of four one-bottle self-etching adhesive systems with Er:YAG laser-irradiated dentin.

PubMed

Jiang, Qianzhou; Chen, Minle; Ding, Jiangfeng

2013-12-01

This study aimed to investigate the interaction of current one-bottle self-etching adhesives and Er:YAG laser with dentin using a tensile bond strength (TBS) test and scanning electron microscopy (SEM) in vitro. Two hundred and thirteen dentin discs were randomly distributed to the Control Group using bur cutting and to the Laser Group using an Er:YAG laser (200 mJ, VSP, 20 Hz). The following adhesives were investigated: one two-step total-etch adhesive [Prime & Bond NT (Dentsply)] and four one-step self-etch adhesives [G-Bond plus (GC), XENO V (Dentsply), iBond Self Etch (Heraeus) and Adper Easy One (3 M ESPE)]. Samples were restored with composite resin, and after 24-hour storage in distilled water, subjected to the TBS test. For morphological analysis, 12 dentin specimens were prepared for SEM. No significant differences were found between the control group and laser group (p = 0.899); dentin subjected to Prime & Bond NT, XENOV and Adper Easy One produced higher TBS. In conclusion, this study indicates that Er:YAG laser-prepared dentin can perform as well as bur on TBS, and some of the one-step one-bottle adhesives are comparable to the total-etch adhesives in TBS on dentin.

Electrodeposited manganese dioxide nanostructures on electro-etched carbon fibers: High performance materials for supercapacitor applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kazemi, Sayed Habib, E-mail: habibkazemi@iasbs.ac.ir; Center for Research in Climate Change and Global Warming; Maghami, Mostafa Ghaem

Highlights: • We report a facile method for fabrication of MnO{sub 2} nanostructures on electro-etched carbon fiber. • MnO{sub 2}-ECF electrode shows outstanding supercapacitive behavior even at high discharge rates. • Exceptional cycle stability was achieved for MnO{sub 2}-ECF electrode. • The coulombic efficiency of MnO{sub 2}-ECF electrode is nearly 100%. - Abstract: In this article we introduce a facile, low cost and additive/template free method to fabricate high-rate electrochemical capacitors. Manganese oxide nanostructures were electrodeposited on electro-etched carbon fiber substrate by applying a constant anodic current. Nanostructured MnO{sub 2} on electro-etched carbon fiber was characterized by scanning electron microscopy,more » X-ray diffraction and energy dispersive X-ray analysis. The electrochemical behavior of MnO{sub 2} electro-etched carbon fiber electrode was investigated by electrochemical techniques including cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy. A maximum specific capacitance of 728.5 F g{sup −1} was achieved at a scan rate of 5 mV s{sup −1} for MnO{sub 2} electro-etched carbon fiber electrode. Also, this electrode showed exceptional cycle stability, suggesting that it can be considered as a good candidate for supercapacitor electrodes.« less

Sculpting the internal architecture of fluorescent silica particles via a template-free approach.

PubMed

Rosu, Cornelia; Gorman, Andrew J; Cueto, Rafael; Dooley, Kerry M; Russo, Paul S

2016-04-01

Particles with an open, porous structure can be used to deliver payloads. It is often of interest to detect such particles in tissue or materials, which is facilitated by addition of dye. A straightforward approach leading to fluorescent, porous silica particles is described. The particles are etched with 3mM aqueous sodium hydroxide, taking advantage of the etching rate difference between normal silica and an interior band of silica that contains covalently attached dye. No additional steps, such as dye labeling or thermal annealing, are required. Etching modeled the internal structure of the fluorescent silica particles by creating meso/macropores and voids, as reflected by nitrogen absorption measurements. In order to investigate whether a polymer shell influences etching, certain composite particles are top-coated with poly(l-lysine) representing neutral or positive charged surfaces under typical pH conditions in living systems. The polypeptide-coated fluorescent silica cores exhibit the same porous morphology as uncoated homologs. The polypeptide topcoat does little to alter the permeation by the etching agent. Preservation of size during etching, confirmed by dynamic light scattering, transmission electron microscopy and small-angle X-ray scattering, simplifies the use of these template-free porous fluorescent particles as platforms for drug encapsulation, drug carriers and in vivo imaging. Copyright © 2016 Elsevier Inc. All rights reserved.

Self-assembly and continuous growth of hexagonal graphene flakes on liquid Cu

NASA Astrophysics Data System (ADS)

Cho, Seong-Yong; Kim, Min-Sik; Kim, Minsu; Kim, Ki-Ju; Kim, Hyun-Mi; Lee, Do-Joong; Lee, Sang-Hoon; Kim, Ki-Bum

2015-07-01

Graphene growth on liquid Cu has received great interest, owing to the self-assembly behavior of hexagonal graphene flakes with aligned orientation and to the possibility of forming a single grain of graphene through a commensurate growth of these graphene flakes. Here, we propose and demonstrate a two-step growth process which allows the formation of self-assembled, completely continuous graphene on liquid Cu. After the formation of full coverage on the liquid Cu, grain boundaries were revealed via selective hydrogen etching and the original grain boundaries were clearly resolved. This result indicates that, while the flakes self-assembled with the same orientation, there still remain structural defects, gaps and voids that were not resolved by optical microscopy or scanning electron microscopy. To overcome this limitation, the two-step growth process was employed, consisting of a sequential process of a normal single-layer graphene growth and self-assembly process with a low carbon flux, followed by the final stage of graphene growth at a high degree of supersaturation with a high carbon flux. Continuity of the flakes was verified via hydrogen etching and a NaCl-assisted oxidation process, as well as by measuring the electrical properties of the graphene grown by the two-step process. Two-step growth can provide a continuous graphene layer, but commensurate stitching should be further studied.Graphene growth on liquid Cu has received great interest, owing to the self-assembly behavior of hexagonal graphene flakes with aligned orientation and to the possibility of forming a single grain of graphene through a commensurate growth of these graphene flakes. Here, we propose and demonstrate a two-step growth process which allows the formation of self-assembled, completely continuous graphene on liquid Cu. After the formation of full coverage on the liquid Cu, grain boundaries were revealed via selective hydrogen etching and the original grain boundaries were clearly resolved. This result indicates that, while the flakes self-assembled with the same orientation, there still remain structural defects, gaps and voids that were not resolved by optical microscopy or scanning electron microscopy. To overcome this limitation, the two-step growth process was employed, consisting of a sequential process of a normal single-layer graphene growth and self-assembly process with a low carbon flux, followed by the final stage of graphene growth at a high degree of supersaturation with a high carbon flux. Continuity of the flakes was verified via hydrogen etching and a NaCl-assisted oxidation process, as well as by measuring the electrical properties of the graphene grown by the two-step process. Two-step growth can provide a continuous graphene layer, but commensurate stitching should be further studied. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03352g

Characterization of Etch Pit Formation via the Everson-Etching Method on CdZnTe Crystal Surfaces from the Bulk to the Nano-Scale

DOE Office of Scientific and Technical Information (OSTI.GOV)

Teague, L.; Duff, M.; Cadieux, J.

2010-09-24

A combination of atomic force microscopy, optical microscopy, and mass spectrometry was employed to study CdZnTe crystal surface and used etchant solution following exposure of the CdZnTe crystal to the Everson etch solution. We discuss the results of these studies in relationship to the initial surface preparation methods, the performance of the crystals as radiation spectrometers, the observed etch pit densities, and the chemical mechanism of surface etching. Our results show that the surface features that are exposed to etchants result from interactions with the chemical components of the etchants as well as pre-existing mechanical polishing.

[Brushing abrasion of the enamel surface after erosion].

PubMed

Lipei, Chen; Xiangke, Ci; Xiaoyan, Ou

2017-08-01

Objective A study was conducted to compare the effect of different enamel remineralization periods after erosion on the depth of brushing abrasion. Methods Ten volunteers were selected for a 4-day experiment. A total of 60 enamels were randomly assigned into six groups (A-F) and placed in intraoral palatal devices. On the first day, the palatal devices were placed in oral cavity (24 h) . On the following three days, brushing experiments were performed extraorally, two times per day. The specific experimental method of brushing follows these next steps. First, the group F specimens were covered with a film of wax, and then acid etched for 2 min. Subsequently, the film of wax was detached. The groups from A to D were brushed after remineralization at the following time intervals: group A, 0 min; group B, 20 min; group C, 40 min; group D, 60 min. Erosion and remineralization were performed on group E, but without brushing. Remineralization was performed on group F, but without acid etching and brushing. The depth of enamel abrasion was determined by a mechanical profilometer. The surface morphology of the enamel blocks was observed using a scanning electron microscope. Results 1) The depth of abrasion was different in varied enamel remineralization time after acid etching. The statistical significant differences between groups were as follows. 2) When the time of enamel remineralization after acid etching was short, the surface depression in the electron microscope was deep, and the surface morphology was rough. Conclusion Brushing immediately after acid etching would cause much serious abrasion to the enamel surface. Brushing after 60 min can effectively reduce the abrasion of acid etching enamel.

Etching of germanium-tin using ammonia peroxide mixture

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dong, Yuan; Ong, Bin Leong; Wang, Wei

The wet etching of germanium-tin (Ge{sub 1-x}Sn{sub x}) alloys (4.2% < x < 16.0%) in ammonia peroxide mixture (APM) is investigated. Empirical fitting of the data points indicates that the etch depth of Ge{sub 1-x}Sn{sub x} is proportional to the square root of the etch time t and decreases exponentially with increasing x for a given t. In addition, X-ray photoelectron spectroscopy results show that increasing t increases the intensity of the Sn oxide peak, whereas no obvious change is observed for the Ge oxide peak. This indicates that an accumulation of Sn oxide on the Ge{sub 1-x}Sn{sub x} surface decreases the amount ofmore » Ge atoms exposed to the etchant, which accounts for the decrease in etch rate with increasing etch time. Atomic force microscopy was used to examine the surface morphologies of the Ge{sub 0.918}Sn{sub 0.082} samples. Both root-mean-square roughness and undulation periods of the Ge{sub 1-x}Sn{sub x} surface were observed to increase with increasing t. This work provides further understanding of the wet etching of Ge{sub 1-x}Sn{sub x} using APM and may be used for the fabrication of Ge{sub 1-x}Sn{sub x}-based electronic and photonic devices.« less

Effect of surface etching on the oxidation behavior of plasma chromizing-treated AISI440B stainless steel

NASA Astrophysics Data System (ADS)

Meng, T. X.; Guo, Q.; Xi, W.; Ding, W. Q.; Liu, X. Z.; Lin, N. M.; Yu, S. W.; Liu, X. P.

2018-03-01

Double glow plasma surface alloying was applied to prepare chromizing layer in the surface of AISI440B stainless steel. Prior to chromizing, the stainless steel was etched by microwave plasma chemical vapor deposition to change the surface morphology and composition, and then heated for chromizing at 950 °C for 3 h. The cyclical oxidation of steel after chromizing was carried out at 900 °C for 100 h. Scanning electron microscopy, glow discharge optical emission spectrometer and X-ray diffractometer were used to characterize microstructure, composition and phase structure of alloyed and oxidized samples. The results show that the surface was composed of the Cr-rich top layer and Cr23C6, Cr7C3 and {Cr,Fe}7C3 below layer after chromizing. The bonding between the chromizing layer and the substrate after etching treatment was obviously strengthened. AISI440B steel shows a poor oxidation resistance and the weight gain oxidized for 100 h was up to 31.1 mg/cm2. Weight gains for chromizing and etching + chromizing treated samples were 0.67 mg/cm2 and 8 mg/cm2, respectively. Both oxidized surfaces of chromizing and etching + chromizing were composed of Cr2O3, but the oxide scale of etching + chromizing treated samples was more compact than that of samples without etching.

Chemical lift-off and direct wafer bonding of GaN/InGaN P-I-N structures grown on ZnO

NASA Astrophysics Data System (ADS)

Pantzas, K.; Rogers, D. J.; Bove, P.; Sandana, V. E.; Teherani, F. H.; El Gmili, Y.; Molinari, M.; Patriarche, G.; Largeau, L.; Mauguin, O.; Suresh, S.; Voss, P. L.; Razeghi, M.; Ougazzaden, A.

2016-02-01

p-GaN/i-InGaN/n-GaN (PIN) structures were grown epitaxially on ZnO-buffered c-sapphire substrates by metal organic vapor phase epitaxy using the industry standard ammonia precursor for nitrogen. Scanning electron microscopy revealed continuous layers with a smooth interface between GaN and ZnO and no evidence of ZnO back-etching. Energy Dispersive X-ray Spectroscopy revealed a peak indium content of just under 5 at% in the active layers. The PIN structure was lifted off the sapphire by selectively etching away the ZnO buffer in an acid and then direct bonded onto a glass substrate. Detailed high resolution transmission electron microscoy and grazing incidence X-ray diffraction studies revealed that the structural quality of the PIN structures was preserved during the transfer process.

Effect of different electrolytes on porous GaN using photo-electrochemical etching

NASA Astrophysics Data System (ADS)

Al-Heuseen, K.; Hashim, M. R.; Ali, N. K.

2011-05-01

This article reports the properties and the behavior of GaN during the photoelectrochemical etching process using four different electrolytes. The measurements show that the porosity strongly depends on the electrolyte and highly affects the surface morphology of etched samples, which has been revealed by scanning electron microscopy (SEM) images. Peak intensity of the photoluminescence (PL) spectra of the porous GaN samples was observed to be enhanced and strongly depend on the electrolytes. Among the samples, there is a little difference in the peak position indicating that the change of porosity has little influence on the PL peak shift, while it highly affecting the peak intensity. Raman spectra of porous GaN under four different solution exhibit phonon mode E 2 (high), A 1 (LO), A 1 (TO) and E 2 (low). There was a red shift in E 2 (high) in all samples, indicating a relaxation of stress in the porous GaN surface with respect to the underlying single crystalline epitaxial GaN. Raman and PL intensities were high for samples etched in H 2SO 4:H 2O 2 and KOH followed by the samples etched in HF:HNO 3 and in HF:C 2H 5OH.

Eliminating dependence of hole depth on aspect ratio by forming ammonium bromide during plasma etching of deep holes in silicon nitride and silicon dioxide

NASA Astrophysics Data System (ADS)

Iwase, Taku; Yokogawa, Kenetsu; Mori, Masahito

2018-06-01

The reaction mechanism during etching to fabricate deep holes in SiN/SiO2 stacks by using a HBr/N2/fluorocarbon-based gas plasma was investigated. To etch SiN and SiO2 films simultaneously, HBr/fluorocarbon gas mixture ratio was controlled to achieve etching selectivity closest to one. Deep holes were formed in the SiN/SiO2 stacks by one-step etching at several temperatures. The surface composition of the cross section of the holes was analyzed by time-of-flight secondary-ion mass spectrometry. It was found that bromine ions (considered to be derived from NH4Br) were detected throughout the holes in the case of low-temperature etching. It was also found that the dependence of hole depth on aspect ratio decreases as temperature decreases, and it becomes significantly weaker at a substrate temperature of 20 °C. It is therefore concluded that the formation of NH4Br supplies the SiN/SiO2 etchant to the bottom of the holes. Such a finding will make it possible to alleviate the decrease in etching rate due to a high aspect ratio.

Atomic force microscopy of atomic-scale ledges and etch pits formed during dissolution of quartz

NASA Technical Reports Server (NTRS)

Gratz, A. J.; Manne, S.; Hansma, P. K.

1991-01-01

The processes involved in the dissolution and growth of crystals are closely related. Atomic force microscopy (AFM) of faceted pits (called negative crystals) formed during quartz dissolution reveals subtle details of these underlying physical mechanisms for silicates. In imaging these surfaces, the AFM detected ledges less than 1 nm high that were spaced 10 to 90 nm apart. A dislocation pit, invisible to optical and scanning electron microscopy measurements and serving as a ledge source, was also imaged. These observations confirm the applicability of ledge-motion models to dissolution and growth of silicates; coupled with measurements of dissolution rate on facets, these methods provide a powerful tool for probing mineral surface kinetics.

Bone cutting capacity and osseointegration of surface-treated orthodontic mini-implants.

PubMed

Kim, Ho-Young; Kim, Sang-Cheol

2016-11-01

The objective of the study was to evaluate the practicality and the validity of different surface treatments of self-drilling orthodontic mini-implants (OMIs) by comparing bone cutting capacity and osseointegration. Self-drilling OMIs were surface-treated in three ways: Acid etched (Etched), resorbable blasting media (RBM), partially resorbabla balsting media (Hybrid). We compared the bone cutting capacity by measuring insertion depths into artificial bone (polyurethane foam). To compare osseointegration, OMIs were placed in the tibia of 25 rabbits and the removal torque value was measured at 1, 2, 4, and 8 weeks after placement. The specimens were analyzed by optical microscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). The bone cutting capacity of the etched and hybrid group was lower than the machined (control) group, and was most inhibited in the RBM group ( p < 0.05). At 4 weeks, the removal torque in the machined group was significantly decreased ( p < 0.05), but was increased in the etched group ( p < 0.05). In the hybrid group, the removal torque significantly increased at 2 weeks, and was the highest among all measured values at 8 weeks ( p < 0.05). The infiltration of bone-like tissue surface was evaluated by SEM, and calcium and phosphorus were detected via EDS only in the hybrid group. Partial RBM surface treatment (hybrid type in this study) produced the most stable self-drilling OMIs, without a corresponding reduction in bone cutting capacity.

Bone cutting capacity and osseointegration of surface-treated orthodontic mini-implants

PubMed Central

Kim, Ho-Young

2016-01-01

Objective The objective of the study was to evaluate the practicality and the validity of different surface treatments of self-drilling orthodontic mini-implants (OMIs) by comparing bone cutting capacity and osseointegration. Methods Self-drilling OMIs were surface-treated in three ways: Acid etched (Etched), resorbable blasting media (RBM), partially resorbabla balsting media (Hybrid). We compared the bone cutting capacity by measuring insertion depths into artificial bone (polyurethane foam). To compare osseointegration, OMIs were placed in the tibia of 25 rabbits and the removal torque value was measured at 1, 2, 4, and 8 weeks after placement. The specimens were analyzed by optical microscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Results The bone cutting capacity of the etched and hybrid group was lower than the machined (control) group, and was most inhibited in the RBM group (p < 0.05). At 4 weeks, the removal torque in the machined group was significantly decreased (p < 0.05), but was increased in the etched group (p < 0.05). In the hybrid group, the removal torque significantly increased at 2 weeks, and was the highest among all measured values at 8 weeks (p < 0.05). The infiltration of bone-like tissue surface was evaluated by SEM, and calcium and phosphorus were detected via EDS only in the hybrid group. Conclusions Partial RBM surface treatment (hybrid type in this study) produced the most stable self-drilling OMIs, without a corresponding reduction in bone cutting capacity. PMID:27896213

Effect of EDTA and phosphoric Acid pretreatment on the bonding effectiveness of self-etch adhesives to ground enamel.

PubMed

Ibrahim, Ihab M; Elkassas, Dina W; Yousry, Mai M

2010-10-01

This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9-1.0), intermediary strong AdheSE (pH=1.6-1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel.

Defying ageing: An expectation for dentine bonding with universal adhesives?

PubMed

Zhang, Zheng-yi; Tian, Fu-cong; Niu, Li-na; Ochala, Kirsten; Chen, Chen; Fu, Bai-ping; Wang, Xiao-yan; Pashley, David H; Tay, Franklin R

2016-02-01

The present study evaluated the long-term dentine bonding effectiveness of five universal adhesives in etch-and-rinse or self-etch mode after 12 months of water-ageing. The adhesives evaluated included All-Bond Universal, Clearfil Universal Bond, Futurabond U Prime&Bond Elect and Scotchbond Universal. Microtensile bond strength and transmission electron microscopy of the resin-dentine interfaces created in human coronal dentine were examined after 24h or 12 months. Microtensile bond strength were significantly affected by bonding strategy (etch-and-rinse vs self-etch) and ageing (24h vs 12 months). All subgroups showed significantly decreased bond strength after ageing except for Prime&Bond Elect and Scotchbond Universal used in self-etch mode. All five adhesives employed in etch-and-rinse mode exhibited ultrastructural features characteristic of collagen degradation and resin hydrolysis. A previously-unobserved inside-out collagen degradation pattern was identified in hybrid layers created by 10-MDP containing adhesives (All-Bond Universal, Scotchbond Universal and Clearfil Universal Bond) in the etch-and-rinse mode, producing partially degraded collagen fibrils with intact periphery and a hollow core. In the self-etch mode, all adhesives except for Prime&Bond Elect exhibited degradation of the collagen fibrils along the thin hybrid layers. The three 10-MDP containing universal adhesives did not protect surface collagen fibrils from degradation when bonding was performed in the self-etch mode. Despite the adjunctive conclusion that bonds created by universal adhesives in the self-etch bonding mode are more resistant to decline in bond strength when compared with those bonds created using the etch-and-rinse mode, bonds created by universal adhesives are generally incapable of defying ageing. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of EDTA and Phosphoric Acid Pretreatment on the Bonding Effectiveness of Self-Etch Adhesives to Ground Enamel

PubMed Central

Ibrahim, Ihab M.; Elkassas, Dina W.; Yousry, Mai M.

2010-01-01

Objectives: This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Methods: Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9–1.0), intermediary strong AdheSE (pH=1.6–1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Results: Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Conclusions: Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel. PMID:20922162

Nanotexturing of polystyrene surface in fluorocarbon plasmas: from sticky to slippery superhydrophobicity.

PubMed

Mundo, Rosa Di; Palumbo, Fabio; d'Agostino, Riccardo

2008-05-06

In this work plasma etching processes have been studied to roughen and fluorinate polystyrene surface as an easy method to achieve a superhydrophobic slippery character. Radiofrequency discharges have been fed with CF(4)/O(2) mixtures and the effect of the O(2):CF(4) ratio, the input power, and the treatment duration have been investigated in terms of wettability, with focus on sliding performances. For this purpose, surface morphological variations, evaluated by means of scanning electron microscopy and atomic force microscopy, together with the chemical assessment by X-ray photoelectron spectroscopy, have been correlated with water contact angle hysteresis and volume resolved sliding angle measurements. Results indicate that by increasing the height and decreasing the density of the structures formed by etching, within a tailored range, a transition from sticky to slippery superhydrophobicity occurs. A short treatment time (5 min) is sufficient to obtain such an effect, provided that a high power input is utilized. Optimized surfaces show a unaltered transparency to visible light according to the low roughness produced.

Characterization of Ag-porous silicon nanostructured layer formed by an electrochemical etching of p-type silicon surface for bio-application

NASA Astrophysics Data System (ADS)

Naddaf, M.; Al-Mariri, A.; Haj-Mhmoud, N.

2017-06-01

Nanostructured layers composed of silver-porous silicon (Ag-PS) have been formed by an electrochemical etching of p-type (1 1 1) silicon substrate in a AgNO3:HF:C2H5OH solution at different etching times (10 min-30 min). Scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS) results reveal that the produced layers consist of Ag dendrites and a silicon-rich porous structure. The nanostructuring nature of the layer has been confirmed by spatial micro-Raman scattering and x-ray diffraction techniques. The Ag dendrites exhibit a surface-enhanced Raman scattering (SERS) spectrum, while the porous structure shows a typical PS Raman spectrum. Upon increasing the etching time, the average size of silicon nanocrystallite in the PS network decreases, while the average size of Ag nanocrystals is slightly affected. In addition, the immobilization of prokaryote Salmonella typhimurium DNA via physical adsorption onto the Ag-PS layer has been performed to demonstrate its efficiency as a platform for detection of biological molecules using SERS.

Determination by Small-angle X-ray Scattering of Pore Size Distribution in Nanoporous Track-etched Polycarbonate Membranes

NASA Astrophysics Data System (ADS)

Jonas, A. M.; Legras, R.; Ferain, E.

1998-03-01

Nanoporous track-etched membranes with narrow pore size distributions and average pore size diameters tunable from 100 to 1000 Åare produced by the chemical etching of latent tracks in polymer films after irradiation by a beam of accelerated heavy ions. Nanoporous membranes are used for highly demanding filtration purposes, or as templates to obtain metallic or polymeric nanowires (L. Piraux et al., Nucl. Instr. Meth. Phys. Res. 1997, B131, 357). Such applications call for developments in nanopore size characterization techniques. In this respect, we report on the characterization by small-angle X-ray scattering (SAXS) of nanopore size distribution (nPSD) in polycarbonate track-etched membranes. The obtention of nPSD requires inverting an ill-conditioned inhomogeneous equation. We present different numerical routes to overcome the amplification of experimental errors in the resulting solutions, including a regularization technique allowing to obtain the nPSD without a priori knowledge of its shape. The effect of deviations from cylindrical pore shape on the resulting distributions are analyzed. Finally, SAXS results are compared to results obtained by electron microscopy and conductometry.

Gold core@silver semishell Janus nanoparticles prepared by interfacial etching.

PubMed

Chen, Limei; Deming, Christopher P; Peng, Yi; Hu, Peiguang; Stofan, Jake; Chen, Shaowei

2016-08-14

Gold core@silver semishell Janus nanoparticles were prepared by chemical etching of Au@Ag core-shell nanoparticles at the air/water interface. Au@Ag core-shell nanoparticles were synthesized by chemical deposition of a silver shell onto gold seed colloids followed by the self-assembly of 1-dodecanethiol onto the nanoparticle surface. The nanoparticles then formed a monolayer on the water surface of a Langmuir-Blodgett trough, and part of the silver shell was selectively etched away by the mixture of hydrogen peroxide and ammonia in the water subphase, where the etching was limited to the side of the nanoparticles that was in direct contact with water. The resulting Janus nanoparticles exhibited an asymmetrical distribution of silver on the surface of the gold cores, as manifested in transmission electron microscopy, UV-vis absorption, and X-ray photoelectron spectroscopy measurements. Interestingly, the Au@Ag semishell Janus nanoparticles exhibited enhanced electrocatalytic activity in oxygen reduction reactions, as compared to their Au@Ag and Ag@Au core-shell counterparts, likely due to a synergistic effect between the gold cores and silver semishells that optimized oxygen binding to the nanoparticle surface.

Effect of purification method of β-chitin from squid pen on the properties of β-chitin nanofibers.

PubMed

Suenaga, Shin; Nikaido, Nozomi; Totani, Kazuhide; Kawasaki, Kazunori; Ito, Yoshihito; Yamashita, Kazuhiko; Osada, Mitsumasa

2016-10-01

The relationship between purification methods of β-chitin from squid pen and the physicochemical properties of β-chitin nanofibers (NFs) were investigated. Two types of β-chitin were prepared, with β-chitin (a→b) subjected to acid treatment for decalcification and then base treatment for deproteinization, while β-chitin (b→a) was treated in the opposite order. These β-chitins were disintegrated into NFs using wet pulverization. The β-chitin (b→a) NF dispersion has higher transmittance and viscosity than the β-chitin (a→b) NF dispersion. For the first time, we succeeded in obtaining 3D images of the β-chitin NF dispersion in water by using quick-freeze deep-etch replication with high-angle annular dark field scanning transmission electron microscopy. The β-chitin (b→a) NF dispersion has a denser and more uniform 3D network structure than the β-chitin (a→b) NF dispersion. Widths of the β-chitin (a→b) and (b→a) NFs were approximately 8-25 and 3-10nm, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of surface roughness and energy on ice adhesion strength

NASA Astrophysics Data System (ADS)

Zou, M.; Beckford, S.; Wei, R.; Ellis, C.; Hatton, G.; Miller, M. A.

2011-02-01

The aim of this study is to investigate the effects of surface roughness and surface energy on ice adhesion strength. Sandblasting technique was used to prepare samples with high roughness. Silicon-doped hydrocarbon and fluorinated-carbon thin films were employed to alter the surface energy of the samples. Silicon-doped hydrocarbon films were deposited by plasma-enhanced chemical vapor deposition, while fluorinated-carbon films were produced using deep reactive ion etching equipment by only activating the passivation step. Surface topographies were characterized using scanning electron microscopy and a stylus profilometer. The surface wetting properties were characterized by a video-based contact angle measurement system. The adhesion strength of ice formed from a water droplet on these surfaces was studied using a custom-built shear force test apparatus. It was found that the ice adhesion strength is correlated to the water contact angles of the samples only for surfaces with similar roughness: the ice adhesion strength decreases with the increase in water contact angle. The study also shows that smoother as-received sample surfaces have lower ice adhesion strength than the much rougher sandblasted surfaces.

Nanometer Scale Titanium Surface Texturing Are Detected by Signaling Pathways Involving Transient FAK and Src Activations

PubMed Central

Zambuzzi, Willian F.; Bonfante, Estevam A.; Jimbo, Ryo; Hayashi, Mariko; Andersson, Martin; Alves, Gutemberg; Takamori, Esther R.; Beltrão, Paulo J.; Coelho, Paulo G.; Granjeiro, José M.

2014-01-01

Background It is known that physico/chemical alterations on biomaterial surfaces have the capability to modulate cellular behavior, affecting early tissue repair. Such surface modifications are aimed to improve early healing response and, clinically, offer the possibility to shorten the time from implant placement to functional loading. Since FAK and Src are intracellular proteins able to predict the quality of osteoblast adhesion, this study evaluated the osteoblast behavior in response to nanometer scale titanium surface texturing by monitoring FAK and Src phosphorylations. Methodology Four engineered titanium surfaces were used for the study: machined (M), dual acid-etched (DAA), resorbable media microblasted and acid-etched (MBAA), and acid-etch microblasted (AAMB). Surfaces were characterized by scanning electron microscopy, interferometry, atomic force microscopy, x-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy. Thereafter, those 4 samples were used to evaluate their cytotoxicity and interference on FAK and Src phosphorylations. Both Src and FAK were investigated by using specific antibody against specific phosphorylation sites. Principal Findings The results showed that both FAK and Src activations were differently modulated as a function of titanium surfaces physico/chemical configuration and protein adsorption. Conclusions It can be suggested that signaling pathways involving both FAK and Src could provide biomarkers to predict osteoblast adhesion onto different surfaces. PMID:24999733

Advanced fabrication of Si nanowire FET structures by means of a parallel approach.

PubMed

Li, J; Pud, S; Mayer, D; Vitusevich, S

2014-07-11

In this paper we present fabricated Si nanowires (NWs) of different dimensions with enhanced electrical characteristics. The parallel fabrication process is based on nanoimprint lithography using high-quality molds, which facilitates the realization of 50 nm-wide NW field-effect transistors (FETs). The imprint molds were fabricated by using a wet chemical anisotropic etching process. The wet chemical etch results in well-defined vertical sidewalls with edge roughness (3σ) as small as 2 nm, which is about four times better compared with the roughness usually obtained for reactive-ion etching molds. The quality of the mold was studied using atomic force microscopy and scanning electron microscopy image data. The use of the high-quality mold leads to almost 100% yield during fabrication of Si NW FETs as well as to an exceptional quality of the surfaces of the devices produced. To characterize the Si NW FETs, we used noise spectroscopy as a powerful method for evaluating device performance and the reliability of structures with nanoscale dimensions. The Hooge parameter of fabricated FET structures exhibits an average value of 1.6 × 10(-3). This value reflects the high quality of Si NW FETs fabricated by means of a parallel approach that uses a nanoimprint mold and cost-efficient technology.

Novel Processes for Modular Integration of Silicon-Germanium MEMS with CMOS Electronics

DTIC Science & Technology

2007-02-28

process limits the compatibility with further lithography steps. Using silicon as the MEMS structural material, most of the integration processes...structures are defined by lithography and deep reactive ion etching. A layer of gasket oxide is deposited as the sacrificial material between the...When the Bragg condition for constructive interference is obtained, a diffraction peak is produced and the relative peak height is proportional to

The effect of SF6 addition in a Cl2/Ar inductively coupled plasma for deep titanium etching

NASA Astrophysics Data System (ADS)

Laudrel, E.; Tillocher, T.; Meric, Y.; Lefaucheux, P.; Boutaud, B.; Dussart, R.

2018-05-01

Titanium is a material of interest for the biomedical field and more particularly for body implantable devices. Titanium deep etching by plasma was carried out in an inductively coupled plasma with a chlorine-based chemistry for the fabrication of titanium-based microdevices. Bulk titanium etch rate was first studied in Cl2/Ar plasma mixture versus the source power and the self-bias voltage. The plasma was characterized by Langmuir probe and by optical emission spectroscopy. The addition of SF6 in the plasma mixture was investigated. Titanium etch rate was optimized and reached a value of 2.4 µm · min-1. The nickel hard mask selectivity was also enhanced. The etched titanium surface roughness was reduced significantly.

Silicon macroporous arrays with high aspect ratio prepared by ICP etching

NASA Astrophysics Data System (ADS)

Wang, Guozheng; Yang, Bingchen; Wang, Ji; Yang, Jikai; Duanmu, Qingduo

2018-02-01

This paper reports on a macroporous silicon arrays with high aspect ratio, the pores of which are of 162, 205, 252, 276μm depths with 6, 10, 15 and 20 μm diameters respectively, prepared by Multiplex Inductively Coupled Plasma (ICP) etching. It was shown that there are very differences in process of high aspect ratio microstructures between the deep pores, a closed structure, and deep trenches, a open structure. The morphology and the aspect ratio dependent etching were analyzed and discussed. The macroporous silicon etched by ICP process yield an uneven, re-entrant, notched and ripples surface within the pores. The main factors effecting on the RIE lag of HARP etching are the passivation cycle time, the pressure of reactive chamber, and the platen power of ICP system.

Quantum dot immunocytochemical localization of somatostatin in somatostatinoma by Widefield Epifluorescence, super-resolution light, and immunoelectron microscopy.

PubMed

Killingsworth, Murray C; Lai, Ken; Wu, Xiaojuan; Yong, Jim L C; Lee, C Soon

2012-11-01

Quantum dot nanocrystal probes (QDs) have been used for detection of somatostatin hormone in secretory granules of somatostatinoma tumor cells by immunofluorescence light microscopy, super-resolution light microscopy, and immunoelectron microscopy. Immunostaining for all modalities was done using sections taken from an epoxy resin-embedded tissue specimen and a similar labeling protocol. This approach allowed assessment of labeling at light microscopy level before examination at super-resolution and electron microscopy level and was a significant aid in interpretation. Etching of ultrathin sections with saturated sodium metaperiodate was a critical step presumably able to retrieve some tissue antigenicity masked by processing in epoxy resin. Immunofluorescence microscopy of QD-immunolabeled sections showed somatostatin hormone localization in cytoplasmic granules. Some variable staining of tumor gland-like structures appeared related to granule maturity and dispersal of granule contents within the tumor cell cytoplasm. Super-resolution light microscopy demonstrated localization of somatostatin within individual secretory granules to be heterogeneous, and this staining pattern was confirmed by immunoelectron microscopy.

Quantum Dot Immunocytochemical Localization of Somatostatin in Somatostatinoma by Widefield Epifluorescence, Super-resolution Light, and Immunoelectron Microscopy

PubMed Central

Lai, Ken; Wu, Xiaojuan; Yong, Jim L. C.; Lee, C. Soon

2012-01-01

Quantum dot nanocrystal probes (QDs) have been used for detection of somatostatin hormone in secretory granules of somatostatinoma tumor cells by immunofluorescence light microscopy, super-resolution light microscopy, and immunoelectron microscopy. Immunostaining for all modalities was done using sections taken from an epoxy resin-embedded tissue specimen and a similar labeling protocol. This approach allowed assessment of labeling at light microscopy level before examination at super-resolution and electron microscopy level and was a significant aid in interpretation. Etching of ultrathin sections with saturated sodium metaperiodate was a critical step presumably able to retrieve some tissue antigenicity masked by processing in epoxy resin. Immunofluorescence microscopy of QD-immunolabeled sections showed somatostatin hormone localization in cytoplasmic granules. Some variable staining of tumor gland-like structures appeared related to granule maturity and dispersal of granule contents within the tumor cell cytoplasm. Super-resolution light microscopy demonstrated localization of somatostatin within individual secretory granules to be heterogeneous, and this staining pattern was confirmed by immunoelectron microscopy. PMID:22899862

Structure of the cell envelope of corynebacteria: importance of the non-covalently bound lipids in the formation of the cell wall permeability barrier and fracture plane.

PubMed

Puech, V; Chami, M; Lemassu, A; Lanéelle, M A; Schiffler, B; Gounon, P; Bayan, N; Benz, R; Daffé, M

2001-05-01

With the recent success of the heterologous expression of mycobacterial antigens in corynebacteria, in addition to the importance of these bacteria in biotechnology and medicine, a better understanding of the structure of their cell envelopes was needed. A combination of molecular compositional analysis, ultrastructural appearance and freeze-etch electron microscopy study was used to arrive at a chemical model, unique to corynebacteria but consistent with their phylogenetic relatedness to mycobacteria and other members of the distinctive suprageneric actinomycete taxon. Transmission electron microscopy and chemical analyses showed that the cell envelopes of the representative strains of corynebacteria examined consisted of (i) an outer layer composed of polysaccharides (primarily a high-molecular-mass glucan and arabinomannans), proteins, which include the mycoloyltransferase PS1, and lipids; (ii) a cell wall glycan core of peptidoglycan-arabinogalactan which may contain other sugar residues and was usually esterified by corynomycolic acids; and (iii) a typical plasma membrane bilayer. Freeze-etch electron microscopy showed that most corynomycolate-containing strains exhibited a main fracture plane in their cell wall and contained low-molecular-mass porins, while the fracture occurred within the plasma membrane of strains devoid of both corynomycolate and pore-forming proteins. Importantly, in most strains, the amount of cell wall-linked corynomycolates was not sufficient to cover the bacterial surface; interestingly, the occurrence of a cell wall fracture plane correlated with the amount of non-covalently bound lipids of the strains. Furthermore, these lipids were shown to spontaneously form liposomes, indicating that they may participate in a bilayer structure. Altogether, the data suggested that the cell wall permeability barrier in corynebacteria involved both covalently linked corynomycolates and non-covalently bound lipids of their cell envelopes.

STRUCTURE OF MEMBRANE HOLES IN OSMOTIC AND SAPONIN HEMOLYSIS

PubMed Central

Seeman, P.; Cheng, D.; Iles, G. H.

1973-01-01

Serial section electron microscopy of hemolysing erythrocytes (fixed at 12 s after the onset of osmotic hemolysis) revealed long slits and holes in the membrane, extending to around 1 µm in length. Many but not all of the slits and holes (about 100–1000 Å wide) were confluent with one another. Ferritin and colloidal gold (added after fixation) only permeated those cells containing membrane defects. No such large holes or slits were seen in saponin-treated erythrocytes, and the membrane was highly invaginated, giving the ghost a scalloped outline. Freeze-etch electron microscopy of saponin-treated membranes revealed 40–50 Å-wide pits in the extracellular surface of the membrane. If these pits represent regions from which cholesterol was extracted, then cholesterol is uniformly distributed over the entire erythrocyte membrane. PMID:4566525

Fast and low power Michelson interferometer thermo-optical switch on SOI.

PubMed

Song, Junfeng; Fang, Q; Tao, S H; Liow, T Y; Yu, M B; Lo, G Q; Kwong, D L

2008-09-29

We designed and fabricated silicon-on-insulator based Michelson interferometer (MI) thermo-optical switches with deep etched trenches for heat-isolation. Switch power was reduced approximately 20% for the switch with deep etched trenches, and the MI saved approximately 50% power than that of the Mach-Zehnder interferometer. 10.6 mW switch power, approximately 42 micros switch time for the MI with deep trenches, 13.14 mW switch power and approximately 34 micros switch time for the MI without deep trenches were achieved.

40 CFR Appendix A to Subpart E of... - Interim Transmission Electron Microscopy Analytical Methods-Mandatory and Nonmandatory-and...

Code of Federal Regulations, 2011 CFR

2011-07-01

... representative of the air entering the abatement site. c. Two field blanks are to be taken by removing the cap... of Sample Data Quality Objectives is shown in the following Table II: EC01AP92.003 C. Sample Shipment... or the Burdette procedure (Ref. 7 of Unit II.J.) ii. Plasma etching of the collapsed filter is...

40 CFR Appendix A to Subpart E of... - Interim Transmission Electron Microscopy Analytical Methods-Mandatory and Nonmandatory-and...

Code of Federal Regulations, 2010 CFR

2010-07-01

... representative of the air entering the abatement site. c. Two field blanks are to be taken by removing the cap... of Sample Data Quality Objectives is shown in the following Table II: EC01AP92.003 C. Sample Shipment... or the Burdette procedure (Ref. 7 of Unit II.J.) ii. Plasma etching of the collapsed filter is...

Detachment of CVD-grown graphene from single crystalline Ni films by a pure gas phase reaction

NASA Astrophysics Data System (ADS)

Zeller, Patrick; Henß, Ann-Kathrin; Weinl, Michael; Diehl, Leo; Keefer, Daniel; Lippmann, Judith; Schulz, Anne; Kraus, Jürgen; Schreck, Matthias; Wintterlin, Joost

2016-11-01

Despite great previous efforts there is still a high need for a simple, clean, and upscalable method for detaching epitaxial graphene from the metal support on which it was grown. We present a method based on a pure gas phase reaction that is free of solvents and polymer supports and avoids mechanical transfer steps. The graphene was grown on 150 nm thick, single crystalline Ni(111) films on Si(111) wafers with YSZ buffer layers. Its quality was monitored by using low energy electron diffraction and scanning tunneling microscopy. The gas phase etching uses a chemical transport reaction, the so-called Mond process, based on the formation of gaseous nickel tetracarbonyl in 1 bar of CO at 75 °C and by adding small amounts of sulfide catalysts. X-ray photoelectron spectroscopy, Raman spectroscopy and scanning electron microscopy were used to characterize the detached graphene. It was found that the method successfully removes the nickel from underneath the graphene layer, so that the graphene lies on the insulating oxide buffer layer. Small residual particles of nickel sulfide and cracks in the obtained graphene layer were identified. The defect concentrations were comparable to graphene samples obtained by wet chemical etching and by the bubbling transfer.

Comparison of Erosion Behavior and Particle Contamination in Mass-Production CF4/O2 Plasma Chambers Using Y2O3 and YF3 Protective Coatings

PubMed Central

Lin, Tzu-Ken; Wang, Wei-Kai; Huang, Shih-Yung; Tasi, Chi-Tsung

2017-01-01

Yttrium fluoride (YF3) and yttrium oxide (Y2O3) protective coatings prepared using an atmospheric plasma spraying technique were used to investigate the relationship between surface erosion behaviors and their nanoparticle generation under high-density plasma (1012–1013 cm−3) etching. As examined by transmission electron microscopy, the Y2O3 and YF3 coatings become oxyfluorinated after exposure to the plasma, wherein the yttrium oxyfluoride film formation was observed on the surface with a thickness of 5.2 and 6.8 nm, respectively. The difference in the oxyfluorination of Y2O3 and YF3 coatings could be attributed to Y–F and Y–O bonding energies. X-ray photoelectron spectroscopy analyses revealed that a strongly fluorinated bonding (Y–F bond) was obtained on the etched surface of the YF3 coating. Scanning electron microscopy and energy dispersive X-ray diffraction analysis revealed that the nanoparticles on the 12-inch wafer are composed of etchant gases and Y2O3. These results indicate that the YF3 coating is a more erosion-resistant material, resulting in fewer contamination particles compared with the Y2O3 coating. PMID:28708079

Surface roughness in XeF{sub 2} etching of a-Si/c-Si(100)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stevens, A.A.E.; Beijerinck, H.C.W.

2005-01-01

Single wavelength ellipsometry and atomic force microscopy (AFM) have been applied in a well-calibrated beam-etching experiment to characterize the dynamics of surface roughening induced by chemical etching of a {approx}12 nm amorphous silicon (a-Si) top layer and the underlying crystalline silicon (c-Si) bulk. In both the initial and final phase of etching, where either only a-Si or only c-Si is exposed to the XeF{sub 2} flux, we observe a similar evolution of the surface roughness as a function of the XeF{sub 2} dose proportional to D(XeF{sub 2}){sup {beta}} with {beta}{approx_equal}0.2. In the transition region from the pure amorphous to themore » pure crystalline silicon layer, we observe a strong anomalous increase of the surface roughness proportional to D(XeF{sub 2}){sup {beta}} with {beta}{approx_equal}1.5. Not only the growth rate of the roughness increases sharply in this phase, also the surface morphology temporarily changes to a structure that suggests a cusplike shape. Both features suggest that the remaining a-Si patches on the surface act effectively as a capping layer which causes the growth of deep trenches in the c-Si. The ellipsometry data on the roughness are corroborated by the AFM results, by equating the thickness of the rough layer to 6 {sigma}, with {sigma} the root-mean-square variation of the AFM's distribution function of height differences. In the AFM data, the anomalous behavior is reflected in a too small value of {sigma} which again suggests narrow and deep surface features that cannot be tracked by the AFM tip. The final phase morphology is characterized by an effective increase in surface area by a factor of two, as derived from a simple bilayer model of the reaction layer, using the experimental etch rate as input. We obtain a local reaction layer thickness of 1.5 monolayer consistent with the 1.7 ML value of Lo et al. [Lo et al., Phys. Rev. B 47, 648 (1993)] that is also independent of surface roughness.« less

Effect of Serum and Insulin Modulation on the Organization and Morphology of Matrix Synthesized by Bovine Corneal Stromal Cells

PubMed Central

Bueno, Ericka M.; Saeidi, Nima; Melotti, Suzanna

2009-01-01

The in vitro production of highly organized collagen fibrils by corneal keratocytes in a three-dimensional scaffold-free culture system presents a unique opportunity for the direct observation of organized matrix formation. The objective of this investigation was to develop such a culture system in a glass substrate (for optical accessibility) and to directly examine the effect of reducing serum and/or increasing insulin on the stratification and secretion of aligned matrix by fourth- to fifth-passage bovine corneal stromal keratocytes. Medium concentrations of 0%, 1%, or 10% fetal bovine serum and 0% or 1% insulin–transferrin–selenium were investigated. High-resolution differential interference contrast microscopy, quick-freeze/deep-etch, and conventional transmission electron microscopy were used to monitor the evolution, morphology, and ultrastructure of the cell–matrix constructs. In a medium containing 1% each of serum and insulin–transferrin–selenium, stromal cells stratified and secreted abundant and locally aligned matrix, generating the thickest cell–matrix constructs (allowing handling with forceps). The results of this study have the potential to significantly advance the field of developmental functional engineering of load-bearing tissues by (i) elucidating cues that modulate in vitro cell secretion of organized matrix and (ii) establishing an optically accessible cell culture system for investigating the mechanism of cell secretion of aligned collagen fibrils. PMID:19480568

Metallographic Preparation of Space Shuttle Reaction Control System Thruster Electron Beam Welds for Electron Backscatter Diffraction

NASA Technical Reports Server (NTRS)

Martinez, James

2011-01-01

A Space Shuttle Reaction Control System (RCS) thruster failed during a firing test at the NASA White Sands Test Facility (WSTF), Las Cruces, New Mexico. The firing test was being conducted to investigate a previous electrical malfunction. A number of cracks were found associated with the fuel closure plate/injector assembly (Fig 1). The firing test failure generated a flight constraint to the launch of STS-133. A team comprised of several NASA centers and other research institutes was assembled to investigate and determine the root cause of the failure. The JSC Materials Evaluation Laboratory was asked to compare and characterize the outboard circumferential electron beam (EB) weld between the fuel closure plate (Titanium 6Al-4V) and the injector (Niobium C-103 alloy) of four different RCS thrusters, including the failed RCS thruster. Several metallographic challenges in grinding/polishing, and particularly in etching were encountered because of the differences in hardness, ductility, and chemical resistance between the two alloys and the bimetallic weld. Segments from each thruster were sectioned from the outboard weld. The segments were hot-compression mounted using a conductive, carbon-filled epoxy. A grinding/polishing procedure for titanium alloys was used [1]. This procedure worked well on the titanium; but a thin, disturbed layer was visible on the niobium surface by means of polarized light. Once polished, each sample was micrographed using bright field, differential interference contrast optical microscopy, and scanning electron microscopy (SEM) using a backscatter electron (BSE) detector. No typical weld anomalies were observed in any of the cross sections. However, areas of large atomic contrast were clearly visible in the weld nugget, particularly along fusion line interfaces between the titanium and the niobium. This prompted the need to better understand the chemistry and microstructure of the weld (Fig 2). Energy Dispersive X-Ray Spectroscopy (EDS) was used to confirm the chemical composition of the variations in contrast in these areas. Niobium alloys generally require exposure to more aggressive chemical reagents than titanium alloys for etching because of niobium s chemical resistance; therefore, the titanium portion of the sample was etched first. A five second immersion in Kroll s reagent revealed a general microstructure on the titanium portion of the sample; however, the titanium heat affected zone closest to the weld, was over-etched due to higher concentrations of refined grains and an increase in eta-phase. The Kroll s etchant also revealed some microstructure in the weld nugget itself; the niobium portion of the sample remained unetched.

Synthesis and Characterization of Silicon Nanowires by Electroless Etching

NASA Astrophysics Data System (ADS)

Bhujel, Rabina; Rizal, Umesh; Agarwal, Amit; Swain, Bhabani S.; Swain, Bibhu P.

2018-02-01

Silicon nanowires (SiNWs) were synthesized by two-step electroless etching of p-type Si (100) wafer and characterized by field emission scanning electron microscopy, UV-Vis spectroscopy, x-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The vibrational signature at 1108 and 2087 cm-1 confirmed SiNWs were passivated by both oxygen and hydrogen atoms. Raman peak at 517 cm-1 indicated crystalline SiNWs with tailing toward redshift due to Fano effect. The Si(2p) and Si(2s) core orbital spectra of SiNWs were found at 99.8 and 150.5 eV, respectively. Moreover, the reflection of SiNWs is minimized to 1 to 5% in the 650-nm wavelength.

Synthesis and electroplating of high resolution insulated carbon nanotube scanning probes for imaging in liquid solutions

PubMed Central

Roberts, N.A.; Noh, J.H.; Lassiter, M.G.; Guo, S.; Kalinin, S.V.; Rack, P.D.

2012-01-01

High resolution and isolated scanning probe microscopy (SPM) is in demand for continued development of energy storage and conversion systems involving chemical reactions at the nanoscale as well as an improved understanding of biological systems. Carbon nanotubes (CNTs) have large aspect ratios and, if leveraged properly, can be used to develop high resolution SPM probes. Isolation of SPM probes can be achieved by deposited a dielectric film and selectively etching at the apex of the probe. In this paper the fabrication of a high resolution and isolated SPM tip is demonstrated using electron beam induced etching of a dielectric film deposited onto an SPM tip with an attached CNT at the apex. PMID:22433664

Synthesis and electroplating of high resolution insulated carbon nanotube scanning probes for imaging in liquid solutions.

PubMed

Roberts, N A; Noh, J H; Lassiter, M G; Guo, S; Kalinin, S V; Rack, P D

2012-04-13

High resolution and isolated scanning probe microscopy (SPM) is in demand for continued development of energy storage and conversion systems involving chemical reactions at the nanoscale as well as an improved understanding of biological systems. Carbon nanotubes (CNTs) have large aspect ratios and, if leveraged properly, can be used to develop high resolution SPM probes. Isolation of SPM probes can be achieved by depositing a dielectric film and selectively etching at the apex of the probe. In this paper the fabrication of a high resolution and isolated SPM tip is demonstrated using electron beam induced etching of a dielectric film deposited onto an SPM tip with an attached CNT at the apex.

Structure and Properties of SiO x Films Prepared by Chemical Etching of Amorphous Alloy Ribbons

NASA Astrophysics Data System (ADS)

Fedorov, V. A.; Berezner, A. D.; Beskrovnyi, A. I.; Fursova, T. N.; Pavlikov, A. V.; Bazhenov, A. V.

2018-04-01

The structure and the physical properties of amorphous SiO x films prepared by chemical etching of an iron-based amorphous ribbon alloy have been studied. The neutron diffraction and also the atomicforce and electron microscopy show that the prepared visually transparent films have amorphous structure, exhibit dielectric properties, and their morphology is similar to that of opals. The samples have been studied by differential scanning calorimetry, Raman and IR spectroscopy before and after their heat treatment. It is found that annealing of the films in air at a temperature of 1273 K leads to a change in their chemical compositions: an amorphous SiO2 compound with inclusions of SiO2 nanocrystals (crystobalite) forms.

Etude fondamentale des mecanismes de gravure par plasma de materiaux de pointe: Application a la fabrication de dispositifs photoniques

NASA Astrophysics Data System (ADS)

Stafford, Luc

Advances in electronics and photonics critically depend upon plasma-based materials processing either for transferring small lithographic patterns into underlying materials (plasma etching) or for the growth of high-quality films. This thesis deals with the etching mechanisms of materials using high-density plasmas. The general objective of this work is to provide an original framework for the plasma-material interaction involved in the etching of advanced materials by putting the emphasis on complex oxides such as SrTiO3, (Ba,Sr)TiO 3 and SrBi2Ta2O9 films. Based on a synthesis of the descriptions proposed by different authors to explain the etching characteristics of simple materials in noble and halogenated plasma mixtures, we propose comprehensive rate models for physical and chemical plasma etching processes. These models have been successfully validated using experimental data published in literature for Si, Pt, W, SiO2 and ZnO. As an example, we have been able to adequately describe the simultaneous dependence of the etch rate on ion and reactive neutral fluxes and on the ion energy. From an exhaustive experimental investigation of the plasma and etching properties, we have also demonstrated that the validity of the proposed models can be extended to complex oxides such as SrTiO3, (Ba,Sr)TiO 3 and SrBi2Ta2O9 films. We also reported for the first time physical aspects involved in plasma etching such as the influence of the film microstructural properties on the sputter-etch rate and the influence of the positive ion composition on the ion-assisted desorption dynamics. Finally, we have used our deep investigation of the etching mechanisms of STO films and the resulting excellent control of the etch rate to fabricate a ridge waveguide for photonic device applications. Keywords: plasma etching, sputtering, adsorption and desorption dynamics, high-density plasmas, plasma diagnostics, advanced materials, photonic applications.

Sample preparation methods for scanning electron microscopy of homogenized Al-Mg-Si billets: A comparative study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Österreicher, Johannes Albert; Kumar, Manoj

Characterization of Mg-Si precipitates is crucial for optimizing the homogenization heat treatment of Al-Mg-Si alloys. Although sample preparation is key for high quality scanning electron microscopy imaging, most common methods lead to dealloying of Mg-Si precipitates. In this article we systematically evaluate different sample preparation methods: mechanical polishing, etching with various reagents, and electropolishing using different electrolytes. We demonstrate that the use of a nitric acid and methanol electrolyte for electropolishing a homogenized Al-Mg-Si alloy prevents the dissolution of Mg-Si precipitates, resulting in micrographs of higher quality. This preparation method is investigated in depth and the obtained scanning electron microscopymore » images are compared with transmission electron micrographs: the shape and size of Mg-Si precipitates appear very similar in either method. The scanning electron micrographs allow proper identification and measurement of the Mg-Si phases including needles with lengths of roughly 200 nm. These needles are β″ precipitates as confirmed by high resolution transmission electron microscopy. - Highlights: •Secondary precipitation in homogenized 6xxx Al alloys is crucial for extrudability. •Existing sample preparation methods for SEM are improvable. •Electropolishing with nitric acid/methanol yields superior quality in SEM. •The obtained micrographs are compared to TEM micrographs.« less

[Influence of different porcelain surface treatment method on the bonding of metal brackets to porcelain].

PubMed

Fan, Cun-Hui; Chen, Jie; Liu, Xin-Qiang; Ma, Xin

2005-08-01

To investigate the influence of different porcelain surface treatment methods on the shear bond strength of metal brackets bonded to porcelain. 80 porcelain facets were divided randomly into two groups according to different adhesive material that was used to bond metal brackets. Adhesive material were Jing-Jin enamel adhesive and light-cured composite resin. Each group was further divided into 4 subgroups according to different surface treatment methods, which were acid etching with 37% phosphoric acid (H3PO4), acid etching with 9.6% hydrofluoric acid (HF), deglazing by grinding and silanating the porcelain surface. All specimens were stored in 37 degrees C water for 24 hours and then the shear bond strength and the porcelain fracture after debonding was determined. The porcelain surfaces after HF etching, H3PO4 etching and deglazing by grinding were examined by scanning electron microscopy respectively. The shear bond strengths in the HF etching groups, the deglazing groups and the silanating groups were much greater than that in the phosphoric etching groups (P < 0.01). Adequate orthodontic bonding strength was achieved both when bonded with light-cured composite resin after deglazing by grinding and when bonded with either of these adhesives after HF etching or surface silanating. There were no differences in the rates of porcelain fractures among groups (P > 0.05). HF etching, deglazing by grinding and silanating can all increase the shear bond strength between metal bracket and porcelain. Surface silanating of porcelain is a better surface treatment when metal brackets bonded to porcelain.

The effects of DRIE operational parameters on vertically aligned micropillar arrays

NASA Astrophysics Data System (ADS)

Miller, Kane; Li, Mingxiao; Walsh, Kevin M.; Fu, Xiao-An

2013-03-01

Vertically aligned silicon micropillar arrays have been created by deep reactive ion etching (DRIE) and used for a number of microfabricated devices including microfluidic devices, micropreconcentrators and photovoltaic cells. This paper delineates an experimental design performed on the Bosch process of DRIE of micropillar arrays. The arrays are fabricated with direct-write optical lithography without photomask, and the effects of DRIE process parameters, including etch cycle time, passivation cycle time, platen power and coil power on profile angle, scallop depth and scallop peak-to-peak distance are studied by statistical design of experiments. Scanning electron microscope images are used for measuring the resultant profile angles and characterizing the scalloping effect on the pillar sidewalls. The experimental results indicate the effects of the determining factors, etch cycle time, passivation cycle time and platen power, on the micropillar profile angles and scallop depths. An optimized DRIE process recipe for creating nearly 90° and smooth surface (invisible scalloping) has been obtained as a result of the statistical design of experiments.

Sputtered gold mask for deep chemical etching of silicon

NASA Technical Reports Server (NTRS)

Pisciotta, B. P.; Gross, C.; Olive, R. S.

1975-01-01

Sputtered mask resists chemical attack from acid and has adherence to withstand prolonged submergence in etch solution without lifting from silicon surface. Even under prolonged etch conditions with significant undercutting, gold mask maintained excellent adhesion to silicon surface and imperviousness to acid.

Microstructure, Morphology, and Nanomechanical Properties Near Fine Holes Produced by Electro-Discharge Machining

NASA Astrophysics Data System (ADS)

Blau, P. J.; Howe, J. Y.; Coffey, D. W.; Trejo, R. M.; Kenik, E. D.; Jolly, B. C.; Yang, N.

2012-08-01

Fine holes in metal alloys are employed for many important technological purposes, including cooling and the precise atomization of liquids. For example, they play an important role in the metering and delivery of fuel to the combustion chambers in energy-efficient, low-emission diesel engines. Electro-discharge machining (EDM) is one process employed to produce such holes. Since the hole shape and bore morphology can affect fluid flow, and holes also represent structural discontinuities in the tips of the spray nozzles, it is important to understand the microstructures adjacent to these holes, the features of the hole walls, and the nanomechanical properties of the material that was in some manner altered by the EDM hole-making process. Several techniques were used to characterize the structure and properties of spray-holes in a commercial injector nozzle. These include scanning electron microscopy, cross sectioning and metallographic etching, bore surface roughness measurements by optical interferometry, scanning electron microscopy, and transmission electron microscopy of recast EDM layers extracted with the help of a focused ion beam.

Formation of dysprosium carbide on the graphite (0001) surface

DOE PAGES

Lii-Rosales, Ann; Zhou, Yinghui; Wallingford, Mark; ...

2017-07-12

When using scanning tunneling microscopy, we characterize a surface carbide that forms such that Dy is deposited on the basal plane of graphite. In order to form carbide islands on terraces, Dy is first deposited at 650–800 K, which forms large metallic islands. Upon annealing at 1000 K, these clusters convert to carbide. Deposition directly at 1000 K is ineffective because nucleation on terraces is inhibited. Reaction is signaled by the fact that each carbide cluster is partially or totally surrounded by an etch pit. The etch pit is one carbon layer deep for most carbide clusters. Carbide clusters aremore » also identifiable by striations on their surfaces. Based on mass balance, and assuming that only the surface layer of carbon is involved in the reaction, the carbide has stoichiometry D y 2 C . This is Dy-rich compared with the most common bulk carbide Dy C 2 , which may reflect limited surface carbon transport to the carbide.« less

Glide of threading edge dislocations after basal plane dislocation conversion during 4H-SiC epitaxial growth

NASA Astrophysics Data System (ADS)

Abadier, Mina; Song, Haizheng; Sudarshan, Tangali S.; Picard, Yoosuf N.; Skowronski, Marek

2015-05-01

Transmission electron microscopy (TEM) and KOH etching were used to analyze the motion of dislocations after the conversion of basal plane dislocations (BPDs) to threading edge dislocations (TEDs) during 4H-SiC epitaxy. The locations of TED etch pits on the epilayer surface were shifted compared to the original locations of BPD etch pits on the substrate surface. The shift of the TED etch pits was mostly along the BPD line directions towards the up-step direction. For converted screw type BPDs, the conversion points were located below the substrate/epilayer interface. The shift distances in the step-flow direction were proportional to the depths of the BPD-TED conversion points below the substrate/epilayer interface. For converted mixed type BPDs, the conversion points were exactly at the interface. Through TEM analysis, it was concluded that the dislocation shift is caused by a combined effect of H2 etching prior to growth and glide of the threading segments during high temperature epitaxy. The TED glide is only possible for converted pure screw type BPDs and could present a viable means for eliminating BPDs from the epilayer during growth by moving the conversion point below the substrate/epilayer interface.

Controllable Si (100) micro/nanostructures by chemical-etching-assisted femtosecond laser single-pulse irradiation

NASA Astrophysics Data System (ADS)

Li, Xiaowei; Xie, Qian; Jiang, Lan; Han, Weina; Wang, Qingsong; Wang, Andong; Hu, Jie; Lu, Yongfeng

2017-05-01

In this study, silicon micro/nanostructures of controlled size and shape are fabricated by chemical-etching-assisted femtosecond laser single-pulse irradiation, which is a flexible, high-throughput method. The pulse fluence is altered to create various laser printing patterns for the etching mask, resulting in the sequential evolution of three distinct surface micro/nanostructures, namely, ring-like microstructures, flat-top pillar microstructures, and spike nanostructures. The characterized diameter of micro/nanostructures reveals that they can be flexibly tuned from the micrometer (˜2 μm) to nanometer (˜313 nm) scales by varying the laser pulse fluence in a wide range. Micro-Raman spectroscopy and transmission electron microscopy are utilized to demonstrate that the phase state changes from single-crystalline silicon (c-Si) to amorphous silicon (a-Si) after single-pulse femtosecond laser irradiation. This amorphous layer with a lower etching rate then acts as a mask in the wet etching process. Meanwhile, the on-the-fly punching technique enables the efficient fabrication of large-area patterned surfaces on the centimeter scale. This study presents a highly efficient method of controllably manufacturing silicon micro/nanostructures with different single-pulse patterns, which has promising applications in the photonic, solar cell, and sensors fields.

Monte Carlo simulations of secondary electron emission due to ion beam milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahady, Kyle; Tan, Shida; Greenzweig, Yuval

We present a Monte Carlo simulation study of secondary electron emission resulting from focused ion beam milling of a copper target. The basis of this study is a simulation code which simulates ion induced excitation and emission of secondary electrons, in addition to simulating focused ion beam sputtering and milling. This combination of features permits the simulation of the interaction between secondary electron emission, and the evolving target geometry as the ion beam sputters material. Previous ion induced SE Monte Carlo simulation methods have been restricted to predefined target geometries, while the dynamic target in the presented simulations makes thismore » study relevant to image formation in ion microscopy, and chemically assisted ion beam etching, where the relationship between sputtering, and its effects on secondary electron emission, is important. We focus on a copper target, and validate our simulation against experimental data for a range of: noble gas ions, ion energies, ion/substrate angles and the energy distribution of the secondary electrons. We then provide a detailed account of the emission of secondary electrons resulting from ion beam milling; we quantify both the evolution of the yield as high aspect ratio valleys are milled, as well as the emission of electrons within these valleys that do not escape the target, but which are important to the secondary electron contribution to chemically assisted ion induced etching.« less

Origin of visible and near-infrared photoluminescence from chemically etched Si nanowires decorated with arbitrarily shaped Si nanocrystals.

PubMed

Ghosh, Ramesh; Giri, P K; Imakita, Kenji; Fujii, Minoru

2014-01-31

Arrays of vertically aligned single crystalline Si nanowires (NWs) decorated with arbitrarily shaped Si nanocrystals (NCs) have been fabricated by a silver assisted wet chemical etching method. Scanning electron microscopy and transmission electron microscopy are performed to measure the dimensions of the Si NWs as well as the Si NCs. A strong broad band and tunable visible (2.2 eV) to near-infrared (1.5 eV) photoluminescence (PL) is observed from these Si NWs at room temperature (RT). Our studies reveal that the Si NCs are primarily responsible for the 1.5-2.2 eV emission depending on the cross-sectional area of the Si NCs, while the large diameter Si/SiOx NWs yield distinct NIR PL consisting of peaks at 1.07, 1.10 and 1.12 eV. The latter NIR peaks are attributed to TO/LO phonon assisted radiative recombination of free carriers condensed in the electron-hole plasma in etched Si NWs observed at RT for the first time. Since the shape of the Si NCs is arbitrary, an analytical model is proposed to correlate the measured PL peak position with the cross-sectional area (A) of the Si NCs, and the bandgap (E(g)) of nanostructured Si varies as E(g) = E(g) (bulk) + 3.58 A(-0.52). Low temperature PL studies reveal the contribution of non-radiative defects in the evolution of PL spectra at different temperatures. The enhancement of PL intensity and red-shift of the PL peak at low temperatures are explained based on the interplay of radiative and non-radiative recombinations at the Si NCs and Si/SiO(x) interface. Time resolved PL studies reveal bi-exponential decay with size correlated lifetimes in the range of a few microseconds. Our results help to resolve a long standing debate on the origin of visible-NIR PL from Si NWs and allow quantitative analysis of PL from arbitrarily shaped Si NCs.

Defect formation during chlorine-based dry etching and their effects on the electronic and structural properties of InP/InAsP quantum wells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Landesman, Jean-Pierre, E-mail: jean-pierre.landesman@univ-rennes1.fr; Jiménez, Juan; Torres, Alfredo

The general objective is the investigation of the defects formed by dry etching tools such as those involved in the fabrication of photonic devices with III–V semiconductors. Emphasis is put on plasma exposures with chlorine-based chemistries. In addition to identifying these defects and describing their effects on the electro-optic and structural properties, the long-term target would be to predict the impact on the parameters of importance for photonic devices, and possibly include these predictions in their design. The work is first centered on explaining the experimental methodology. This methodology starts with the design and growth of a quantum well structuremore » on indium phosphide, including ternary indium arsenide/phosphide quantum wells with graded arsenic/phosphor composition. These samples have then been characterized by luminescence methods (photo- and cathodoluminescence), high-resolution transmission electron microscopy, and secondary ion mass spectrometry. As one of the parameters of importance in this study, the authors have also included the doping level. The samples have been exposed to the etching plasmas for “short” durations that do not remove completely the quantum wells, but change their optical signature. No masking layer with lithographic features was involved as this work is purely oriented to study the interaction between the plasma and the samples. A significant difference in the luminescence spectra of the as-grown undoped and doped samples is observed. A mechanism describing the effect of the built-in electric field appearing as a consequence of the doping profile is proposed. This mechanism involves quantum confined Stark effect and electric-field induced carrier escape from the quantum wells. In the following part, the effects of exposure to various chlorine-based plasmas were explored. Differences are again observed between the undoped and doped samples, especially for chemistries containing silicon tetrachloride. Secondary ion mass spectrometry indicates penetration of chlorine in the structures. Transmission electron microscopy is used to characterize the quantum well structure before and after plasma bombardment. By examining carefully the luminescence spectral properties, the authors could demonstrate the influence of the etching plasmas on the built-in electric field (in the case of doped samples), and relate it to some ionic species penetrating the structures. Etching plasmas involving both chlorine and nitrogen have also been studied. The etching rate for these chemistries is much slower than for some of the silicon tetrachloride based chemistries. Their effects on the samples are also very different, showing much reduced effect on the built-in electric field (for the doped samples), but significant blue-shifts of the luminescence peaks that the authors attributed to the penetration of nitrogen in the structures. Nitrogen, in interstitial locations, induces mechanical compressive stress that accounts for the blue-shifts. Finally, from the comparison between secondary ion mass spectrometry and luminescence spectra, the authors suggest some elements for a general mechanism involved in the etching by chloride-chemistries, in which a competition takes place between the species at the surface, active for the etching mechanism, and the species that penetrate the structure, lost for the etching process, but relevant in terms of impact on the electro-optic and structural features of the exposed materials.« less

In vitro extracellular recording and stimulation performance of nanoporous gold-modified multi-electrode arrays.

PubMed

Kim, Yong Hee; Kim, Gook Hwa; Kim, Ah Young; Han, Young Hwan; Chung, Myung-Ae; Jung, Sang-Don

2015-12-01

Nanoporous gold (Au) structures can reduce the impedance and enhance the charge injection capability of multi-electrode arrays (MEAs) used for interfacing neuronal networks. Even though there are various nanoporous Au preparation techniques, fabrication of MEA based on low-cost electro-codeposition of Ag:Au has not been performed. In this work, we have modified a Au MEA via the electro-codeposition of Ag:Au alloy, followed by the chemical etching of Ag, and report on the in vitro extracellular recording and stimulation performance of the nanoporous Au-modified MEA. Ag:Au alloy was electro-codeposited on a bilayer lift-off resist sputter-deposition passivated Au MEA followed by chemical etching of Ag to form a porous Au structure. The porous Au structure was analyzed by scanning electron microscopy and tunneling electron microscopy and found to have an interconnected nanoporous Au structure. The impedance value of the nanoporous Au-modified MEA is 15.4 ± 0.55 kΩ at 1 kHz, accompanied by the base noise V rms of 2.4 ± 0.3 μV. The charge injection limit of the nanoporous Au-modified electrode estimated from voltage transient measurement is approximately 1 mC cm(-2), which is comparable to roughened platinum and carbon nanotube electrodes. The charge injection capability of the nanoporous Au-modified MEA was confirmed by observing stimulus-induced spikes at above 0.2 V. The nanoporous Au-modified MEA showed mechanical durability upon ultrasonic treatment for up to an hour. Electro-codeposition of Ag:Au alloy combined with chemical etching Ag is a low-cost process for fabricating nanoporous Au-modified MEA suitable for establishing the stimulus-response relationship of cultured neuronal networks.

In vitro extracellular recording and stimulation performance of nanoporous gold-modified multi-electrode arrays

NASA Astrophysics Data System (ADS)

Kim, Yong Hee; Kim, Gook Hwa; Kim, Ah Young; Han, Young Hwan; Chung, Myung-Ae; Jung, Sang-Don

2015-12-01

Objective. Nanoporous gold (Au) structures can reduce the impedance and enhance the charge injection capability of multi-electrode arrays (MEAs) used for interfacing neuronal networks. Even though there are various nanoporous Au preparation techniques, fabrication of MEA based on low-cost electro-codeposition of Ag:Au has not been performed. In this work, we have modified a Au MEA via the electro-codeposition of Ag:Au alloy, followed by the chemical etching of Ag, and report on the in vitro extracellular recording and stimulation performance of the nanoporous Au-modified MEA. Approach. Ag:Au alloy was electro-codeposited on a bilayer lift-off resist sputter-deposition passivated Au MEA followed by chemical etching of Ag to form a porous Au structure. Main results. The porous Au structure was analyzed by scanning electron microscopy and tunneling electron microscopy and found to have an interconnected nanoporous Au structure. The impedance value of the nanoporous Au-modified MEA is 15.4 ± 0.55 kΩ at 1 kHz, accompanied by the base noise V rms of 2.4 ± 0.3 μV. The charge injection limit of the nanoporous Au-modified electrode estimated from voltage transient measurement is approximately 1 mC cm-2, which is comparable to roughened platinum and carbon nanotube electrodes. The charge injection capability of the nanoporous Au-modified MEA was confirmed by observing stimulus-induced spikes at above 0.2 V. The nanoporous Au-modified MEA showed mechanical durability upon ultrasonic treatment for up to an hour. Significance. Electro-codeposition of Ag:Au alloy combined with chemical etching Ag is a low-cost process for fabricating nanoporous Au-modified MEA suitable for establishing the stimulus-response relationship of cultured neuronal networks.

Bonding characteristics of self-etching adhesives to intact versus prepared enamel.

PubMed

Perdigão, Jorge; Geraldeli, Saulo

2003-01-01

This study tested the null hypothesis that the preparation of the enamel surface would not affect the enamel microtensile bond strengths of self-etching adhesive materials. Ten bovine incisors were trimmed with a diamond saw to obtain a squared enamel surface with an area of 8 x 8 mm. The specimens were randomly assigned to five adhesives: (1) ABF (Kuraray), an experimental two-bottle self-etching adhesive; (2) Clearfil SE Bond (Kuraray), a two-bottle self-etching adhesive; (3) One-Up Bond F (Tokuyama), an all-in-one adhesive; (4) Prompt L-Pop (3M ESPE), an all-in-one adhesive; and (5) Single Bond (3M ESPE), a two-bottle total-etch adhesive used as positive control. For each specimen, one half was roughened with a diamond bur for 5 seconds under water spray, whereas the other half was left unprepared. The adhesives were applied as per manufacturers' directions. A universal hybrid composite resin (Filtek Z250, 3M ESPE) was inserted in three layers of 1.5 mm each and light-cured. Specimens were sectioned in X and Y directions to obtain bonded sticks with a cross-sectional area of 0.8 +/- 0.2 mm2. Sticks were tested in tension in an Instron at a cross-speed of 1 mm per minute. Statistical analysis was carried out with two-way analysis of variance and Duncan's test at p < .05. Ten extra specimens were processed for observation under a field-emission scanning electron microscope. Single Bond, the total-etch adhesive, resulted in statistically higher microtensile bond strength than any of the other adhesives regardless of the enamel preparation (unprepared = 31.5 MPa; prepared = 34.9 MPa, not statistically different at p < .05). All the self-etching adhesives resulted in higher microtensile bond strength when enamel was roughened than when enamel was left unprepared. However, for ABF and for Clearfil SE Bond this difference was not statistically significant at p > .05. When applied to ground enamel, mean bond strengths of Prompt L-Pop were not statistically different from those of Clearfil SE Bond and ABF. One-Up Bond F did not bond to unprepared enamel. Commercial self-etching adhesives performed better on prepared enamel than on unprepared enamel. The field-emission scanning electron microscope revealed a deep interprismatic etching pattern for the total-etch adhesive, whereas the self-etching systems resulted in an etching pattern ranging from absent to moderate.

Scalloping minimization in deep Si etching on Unaxis DSE tools

NASA Astrophysics Data System (ADS)

Lai, Shouliang; Johnson, Dave J.; Westerman, Russ J.; Nolan, John J.; Purser, David; Devre, Mike

2003-01-01

Sidewall smoothness is often a critical requirement for many MEMS devices, such as microfludic devices, chemical, biological and optical transducers, while fast silicon etch rate is another. For such applications, the time division multiplex (TDM) etch processes, so-called "Bosch" processes are widely employed. However, in the conventional TDM processes, rough sidewalls result due to scallop formation. To date, the amplitude of the scalloping has been directly linked to the silicon etch rate. At Unaxis USA Inc., we have developed a proprietary fast gas switching technique that is effective for scalloping minimization in deep silicon etching processes. In this technique, process cycle times can be reduced from several seconds to as little as a fraction of second. Scallop amplitudes can be reduced with shorter process cycles. More importantly, as the scallop amplitude is progressively reduced, the silicon etch rate can be maintained relatively constant at high values. An optimized experiment has shown that at etch rate in excess of 7 μm/min, scallops with length of 116 nm and depth of 35 nm were obtained. The fast gas switching approach offers an ideal manufacturing solution for MEMS applications where extremely smooth sidewall and fast etch rate are crucial.

Use of hydrogen etching to remove existing dislocations in GaN epitaxial layers

NASA Astrophysics Data System (ADS)

Yeh, Yen-Hsien; Chu, Chung-Ming; Wu, Yin-Hao; Hsu, Ying-Chia; Yu, Tzu-Yi; Lee, Wei-I.

2015-08-01

In this paper, based on the anisotropic nature of hydrogen (H2) etching on GaN, we describe a new approach to the removal of threading dislocations in GaN layers. The top surfaces of c-plane (Ga-face) and a-plane GaNs are considered stable in H2; therefore, H2 etches only crystal imperfections such as dislocation and basal plane stacking fault (BSF) sites. We used H2 to etch undoped c-plane GaN, n-type c-plane GaN, a-plane GaN, and an InGaN/GaN multiple quantum well structure. Several examinations were performed, indicating deep cavities on the c-plane GaN samples after H2 etching; furthermore, gorge-like grooves were observed on the a-plane GaN samples. The deep cavities on the c-plane GaN were considered the etched dislocation sites, and the gorge-like grooves on the a-plane GaN were considered the etched BSF sites. Photoluminescence measurements were performed and the results indicated that the H2-etched samples demonstrate superior optoelectronic properties, probably because of the elimination of dislocations.

Freeze-fracture scanning electron microscopy of Lemna minor L. (duckweed)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Echlin, P.; Pawley, J.B.; Hayes, T.L.

1979-01-01

A detailed study has been carried out on the frozen fracture faces of plant material. Roots of Lemna minor are encapsulated in different nonpenetrating polymeric cryoprotectants, rapidly cooled in melting nitrogen and transferred to the pre-cooled cold stage of the AMR Biochamber. The technique has been used to follow the course of development of the phloem tissue in the root tip. These studies have shown that the phloem parenchyma appears to develop in a regular sequence. Unetched surfaces are virtually featureless, and it is necessary to remove a surface layer of water in order to visualize the biological structure. Themore » amount of water sublimed from the fractured surface is a function of both the time of etching and the water binding capacity of the cell contents. It is not possible to etch cells infiltrated with a penetrating cryoprotectant as the glycerol-water eutectic is stable at low temperatures and no water is lost from the fractured surface. Several distinct stages have been observed during the etching process.« less

Photoluminescence Study of Plasma-Induced Damage of GaInN Single Quantum Well

NASA Astrophysics Data System (ADS)

Izumi, Shouichiro; Minami, Masaki; Kamada, Michiru; Tatsumi, Tetsuya; Yamaguchi, Atsushi A.; Ishikawa, Kenji; Hori, Masaru; Tomiya, Shigetaka

2013-08-01

Plasma-induced damage (PID) due to Cl2/SiCl4/Ar plasma etching of the GaN capping layer (CAP)/GaInN single quantum well (SQW)/GaN structure was investigated by conventional photoluminescence (PL), transmission electron microscopy (TEM), and time-resolved and temperature-dependent photoluminescence (TRPL). SQW PL intensity remained constant initially, although plasma etching of the CAP layer proceeded, but when the etching thickness reached a certain amount (˜60 nm above the SQW), PL intensity started to decrease sharply. On the other hand, TEM observations show that the physical damage (structural damage) was limited to the topmost surface region. These findings can be explained by the results of TRPL studies, which revealed that there exist two different causes of PID. One is an increase in the number of nonradiative recombination centers, which mainly affects the PL intensity. The other is an increase in the quantum level fluctuation owing mainly to physical damage.

Porous carbon-free SnSb anodes for high-performance Na-ion batteries

NASA Astrophysics Data System (ADS)

Choi, Jeong-Hee; Ha, Choong-Wan; Choi, Hae-Young; Seong, Jae-Wook; Park, Cheol-Min; Lee, Sang-Min

2018-05-01

A simple melt-spinning/chemical-etching process is developed to create porous carbon-free SnSb anodes. Sodium ion batteries (SIBs) incorporating these anodes exhibit excellent electrochemical performances by accomodating large volume changes during repeated cycling. The porous carbon-free SnSb anode produced by the melt-spinning/chemical-etching process shows a high reversible capacity of 481 mAh g-1, high ICE of 80%, stable cyclability with a high capacity retention of 99% after 100 cycles, and a fast rate capability of 327 mAh g-1 at 4C-rate. Ex-situ X-ray diffraction and high resolution-transmission electron microscopy analyses demonstrate that the synthesized porous carbon-free SnSb anodes involve the highly reversible reaction with sodium through the conversion and recombination reactions during sodiation/desodiation process. The novel and simple melt-spinning/chemical-etching synthetic process represents a technological breakthrough in the commercialization of Na alloy-able anodes for SIBs.

Surface conditions of Nitinol wires, tubing, and as-cast alloys. The effect of chemical etching, aging in boiling water, and heat treatment.

PubMed

Shabalovskaya, S A; Anderegg, J; Laab, F; Thiel, P A; Rondelli, G

2003-04-15

The surface conditions of Nitinol wires and tubing were evaluated with the use of X-ray photoelectron spectroscopy, high-resolution Auger spectroscopy, electron backscattering, and scanning-electron microscopy. Samples were studied in the as-received state as well as after chemical etching, aging in boiling water, and heat treatment, and compared to a mechanically polished 600-grit-finish Nitinol surface treated similarly. General regularities in surface behavior induced by the examined surface treatments are similar for wires, tubing, and studied as-cast alloy, though certain differences in surface Ni concentration were observed. Nitinol wires and tubing from various suppliers demonstrated great variability in Ni surface concentration (0.5-15 at.%) and Ti/Ni ratio (0.4-35). The wires in the as-received state, with the exception of those with a black oxide originating in the processing procedure, revealed nickel and titanium on the surface in both elemental and oxidized states, indicating a nonpassive surface. Shape-setting heat treatment at 500 degrees C for 15 min resulted in tremendous increase in the surface Ni concentration and complete Ni oxidation. Preliminary chemical etching and boiling in water successfully prevented surface enrichment in Ni, initially resulting from heat treatment. A stoichiometric uniformly amorphous TiO(2) oxide generated during chemical etching and aging in boiling water was reconstructed at 700 degrees C, revealing rutile structure. Copyright 2003 Wiley Periodicals, Inc.

MITLL Silicon Integrated Photonics Process: Design Guide

DTIC Science & Technology

2015-07-31

Silicon Integrated Photonics Process Comprehensive Design Guide 16  Deep Etch for Fiber Coupling (DEEP_ETCH...facets for fiber coupling. Standard design layers for each process are defined in Section 3, but other options can be made available. Notes on...a silicon thinning process that can create very low loss waveguides (and which better suppresses back scatter and, therefore, resonance splitting in

Morphology and electronic properties of silicon carbide surfaces

NASA Astrophysics Data System (ADS)

Nie, Shu

2007-12-01

Several issues related to SiC surfaces are studied in the thesis using scanning tunneling microscopy/spectroscopy (STM/S) and atomic force microscopy (AFM). Specific surfaces examined include electropolished SiC, epitaxial graphene on SiC, and vicinal (i.e. slightly miscut from a low-index direction) SiC that have been subjected to high temperature hydrogen-etching. The electropolished surfaces are meant to mimic electrochemically etched SiC, which forms a porous network. The chemical treatment of the surface is similar between electropolishing and electrochemical etching, but the etching conditions are slightly different such that the former produces a flat surface (that is amenable to STM study) whereas the latter produces a complex 3-dimensional porous network. We have used these porous SiC layers as semi-permeable membranes in a biosensor, and we find that the material is quite biocompatible. The purpose of the STM/STS study is to investigate the surface properties of the SiC on the atomic scale in an effort to explain this biocompatibility. The observed tunneling spectra are found to be very asymmetric, with a usual amount of current at positive voltages but no observable current at negative voltages. We propose that this behavior is due to surface charge accumulating on an incompletely passivated surface. Measurements on SiC surfaces prepared by various amounts of hydrogen-etching are used to support this interpretation. Comparison with tunneling computations reveals a density of about 10 13 cm-2 fixed charges on both the electro-polished and the H-etched surfaces. The relatively insulating nature observed on the electro-polished SiC surface may provide an explanation for the biocompatibility of the surface. Graphene, a monolayer of carbon, is a new material for electronic devices. Epitaxial graphene on SiC is fabricated by the Si sublimation method in which a substrate is heated up to about 1350°C in ultra-high vacuum (UHV). The formation of the graphene is monitored using low-energy electron diffraction (LEED) and Auger electron spectroscopy, and the morphology of the graphitized surface is studied using AFM and STM. Use of H-etched SiC substrates enables a relatively flat surface morphology, although residual steps remain due to unintentional miscut of the wafers. Additionally, some surface roughness in the form of small pits is observed, possibly due to the fact that the surface treatments (H-etching and UHV annealing) having been performed in separate vacuum chambers with an intervening transfer through air. Field-effect transistors have been fabricated with our graphene layers; they show a relatively strong held effect at room temperature, with an electron mobility of 535 cm 2/Vs. This value is somewhat lower than that believed to be theoretically possible for this material, and one possible reason may be the nonideal morphology of the surface (i.e. because of the observed steps and pits). Tunneling spectra of the graphene reveal semi-metallic behavior, consistent with that theoretically expected for an isolated layer of graphene. However, additional discrete states are observed in the spectra, possibly arising from bonding at the graphene/SiC interface. The observation of these states provides important input towards an eventual determination of the complete interface structure, and additionally, such states may be relevant in determining the electron mobility of the graphene. Stepped vicinal SIC{0001} substrates are useful templates for epitaxial growth of various types of layers: thick layers of compound semiconductor (in which the steps help preserving the stacking arrangement in the overlayer), monolayers of graphene, or submonolayer semiconductor layers that form quantum wires along the step edges. Step array produced by H-etching of vicinal SiC (0001) and (0001¯) with various miscut angles have been studied by AFM. H-etching is found to produce full unit-cell-high steps on the (0001) Si-face surfaces, but half unit-cell-high steps on the (0001¯) C-face surfaces. These observations are consistent with an asymmetry in the surface energy (i.e. etch rate) of the two types of step terminations occurring on the different surfaces. For high miscut angles, facet formation is observed on the vicinal Si-face, but less so on the C-face. This difference is interpreted in terms of a lower surface energy of the C-face. In terms of applying the stepped surfaces as a template, a much better uniformity in the step-step separation is found for the C-face surfaces.

Electrochemical Growth of Single-Crystal Metal Nanowires via a Two-Dimensional Nucleation and Growth Mechanism.

PubMed

Tian, Mingliang; Wang, Jinguo; Kurtz, James; Mallouk, Thomas E; Chan, M H W

2003-07-01

Metallic nanowires (Au, Ag, Cu, Ni, Co, and Rh) with an average diameter of 40 nm and a length of 3-5 μm have been fabricated by electrodeposition in the pores of track-etched polycarbonate membranes. Structural characterizations by transmission electron microscopy (TEM) and electron diffraction showed that nanowires of Au, Ag, and Cu are single-crystalline with a preferred [111] orientation, whereas Ni, Co, and Rh wires are polycrystalline. Possible mechanisms responsible for nucleation and growth for single-crystal noble metals versus polycrystalline group VIII-B metals are discussed.

Sea urchin spine calcite forms via a transient amorphous calcium carbonate phase.

PubMed

Politi, Yael; Arad, Talmon; Klein, Eugenia; Weiner, Steve; Addadi, Lia

2004-11-12

The skeletons of adult echinoderms comprise large single crystals of calcite with smooth convoluted fenestrated morphologies, raising many questions about how they form. By using water etching, infrared spectroscopy, electron diffraction, and environmental scanning electron microscopy, we show that sea urchin spine regeneration proceeds via the initial deposition of amorphous calcium carbonate. Because most echinoderms produce the same type of skeletal material, they probably all use this same mechanism. Deposition of transient amorphous phases as a strategy for producing single crystals with complex morphology may have interesting implications for the development of sophisticated materials.

Ultrastructure of the surface of dental enamel with molar incisor hypomineralization (MIH) with and without acid etching.

PubMed

Bozal, Carola B; Kaplan, Andrea; Ortolani, Andrea; Cortese, Silvina G; Biondi, Ana M

2015-01-01

The aim of the present work was to analyze the ultrastructure and mineral composition of the surface of the enamel on a molar with MIH, with and without acid etching. A permanent tooth without clinical MIH lesions (control) and a tooth with clinical diagnosis of mild and moderate MIH, with indication for extraction, were processed with and without acid etching (H3PO4 37%, 20") for observation with scanning electron microscope (SEM) ZEISS (Supra 40) and mineral composition analysis with an EDS detector (Oxford Instruments). The control enamel showed normal prismatic surface and etching pattern. The clinically healthy enamel on the tooth with MIH revealed partial loss of prismatic pattern. The mild lesion was porous with occasional cracks. The moderate lesion was more porous, with larger cracks and many scales. The mineral composition of the affected surfaces had lower Ca and P content and higher O and C. On the tooth with MIH, even on normal looking enamel, the demineralization does not correspond to an etching pattern, and exhibits exposure of crystals with rods with rounded ends and less demineralization in the inter-prismatic spaces. Acid etching increased the presence of cracks and deep pores in the adamantine structure of the enamel with lesion. In moderate lesions, the mineral composition had higher content of Ca, P and Cl. Enamel with MIH, even on clinically intact adamantine surfaces, shows severe alterations in the ultrastructure and changes in ionic composition, which affect the acid etching pattern and may interfere with adhesion.

Pulsed Laser-Assisted Focused Electron-Beam-Induced Etching of Titanium with XeF 2 : Enhanced Reaction Rate and Precursor Transport

DOE PAGES

Noh, J. H.; Fowlkes, J. D.; Timilsina, R.; ...

2015-01-28

We introduce a laser-assisted focused electron-beam-induced etching (LA-FEBIE) process which is a versatile, direct write nanofabrication method that allows nanoscale patterning and editing; we do this in order to enhance the etch rate of electron-beam-induced etching. The results demonstrate that the titanium electron stimulated etch rate via the XeF2 precursor can be enhanced up to a factor of 6 times with an intermittent pulsed laser assist. Moreover, the evolution of the etching process is correlated to in situ stage current measurements and scanning electron micrographs as a function of time. Finally, the increased etch rate is attributed to photothermally enhancedmore » Ti–F reaction and TiF4 desorption and in some regimes enhanced XeF2 surface diffusion to the reaction zone.« less

Cutoff-mesa isolated rib optical waveguide for III-V heterostructure photonic integrated circuits

DOEpatents

Vawter, Gregory A.; Smith, Robert E.

1998-01-01

A cutoff mesa rib waveguide provides single-mode performance regardless of any deep etches that might be used for electrical isolation between integrated electrooptic devices. Utilizing a principle of a cutoff slab waveguide with an asymmetrical refractive index profile, single mode operation is achievable with a wide range of rib widths and does not require demanding etch depth tolerances. This new waveguide design eliminates reflection effects, or self-interference, commonly seen when conventional rib waveguides are combined with deep isolation etches and thereby reduces high order mode propagation and crosstalk compared to the conventional rib waveguides.

Cutoff-mesa isolated rib optical waveguide for III-V heterostructure photonic integrated circuits

DOEpatents

Vawter, G.A.; Smith, R.E.

1998-04-28

A cutoff mesa rib waveguide provides single-mode performance regardless of any deep etches that might be used for electrical isolation between integrated electrooptic devices. Utilizing a principle of a cutoff slab waveguide with an asymmetrical refractive index profile, single mode operation is achievable with a wide range of rib widths and does not require demanding etch depth tolerances. This new waveguide design eliminates reflection effects, or self-interference, commonly seen when conventional rib waveguides are combined with deep isolation etches and thereby reduces high order mode propagation and crosstalk compared to the conventional rib waveguides. 7 figs.

Performance of a new one-step multi-mode adhesive on etched vs non-etched enamel on bond strength and interfacial morphology.

PubMed

de Goes, Mario Fernando; Shinohara, Mirela Sanae; Freitas, Marcela Santiago

2014-06-01

To compare microtensile bond strength (μTBS) and interfacial morphology of a new one-step multimode adhesive with a two-step self-etching adhesive and two etch-and-rinse adhesives systems on enamel. Thirty human third molars were sectioned to obtain two enamel fragments. For μTBS, 48 enamel surfaces were ground using 600-grit SiC paper and randomly assigned into 6 groups (n = 8): nonetched Scotchbond Universal [SBU]; etched SBU [SBU-et]; non-etched Clearfil SE Bond [CSE]; etched CSE [CSE-et]; Scotchbond Multi-PURPOSE [SBMP]; Excite [EX]. The etched specimens were conditioned with 37% phosphoric acid for 30 s, each adhesive system was applied according to manufacturers' instructions, and composite resin blocks (Filtek Supreme Plus, 3M ESPE) were incrementally built up. Specimens were sectioned into beams with a cross-sectional area of 0.8-mm2 and tested under tension (1 mm/min). The data were analyzed with oneway ANOVA and Fisher's PLSD (α = 0.05). For interface analysis, two samples from each group were embedded in epoxy resin, polished, and then observed using scanning electron microscopy (SEM). The μTBS values (in MPa) and the standard deviations were: SBU = 27.4 (8.5); SBU-et = 33.6 (9.3); CSE = 28.5 (8.3); CSE-et = 34.2 (9.0); SBMP = 30.4 (11.0); EX = 23.3 (8.2). CSE-et and SBU-et presented the highest bond strength values, followed by SBMP, CSE, and SBU which did not differ significantly from each other. EX showed the statistically significantly lowest bond strength values. SEM images of interfaces from etched samples showed long adhesive-resin tags penetrating into demineralized enamel. Preliminary etching of enamel significantly increased bond strength for the new one-step multimode adhesive SBU and two-step self-etching adhesive CSE.

Enhancing elastic stress relaxation in SiGe/Si heterostructures by Si pillar necking

NASA Astrophysics Data System (ADS)

Isa, F.; Salvalaglio, M.; Arroyo Rojas Dasilva, Y.; Jung, A.; Isella, G.; Erni, R.; Timotijevic, B.; Niedermann, P.; Gröning, P.; Montalenti, F.; von Känel, H.

2016-10-01

We demonstrate that the elastic stress relaxation mechanism in micrometre-sized, highly mismatched heterostructures may be enhanced by employing patterned substrates in the form of necked pillars, resulting in a significant reduction of the dislocation density. Compositionally graded Si1-xGex crystals were grown by low energy plasma enhanced chemical vapour deposition, resulting in tens of micrometres tall, three-dimensional heterostructures. The patterned Si(001) substrates consist of micrometre-sized Si pillars either with the vertical {110} or isotropically under-etched sidewalls resulting in narrow necks. The structural properties of these heterostructures were investigated by defect etching and transmission electron microscopy. We show that the dislocation density, and hence the competition between elastic and plastic stress relaxation, is highly influenced by the shape of the substrate necks and their proximity to the mismatched epitaxial material. The SiGe dislocation density increases monotonically with the crystal width but is significantly reduced by the substrate under-etching. The drop in dislocation density is interpreted as a direct effect of the enhanced compliance of the under-etched Si pillars, as confirmed by the three-dimensional finite element method simulations of the elastic energy distribution.

Polarity-inverted lateral overgrowth and selective wet-etching and regrowth (PILOSWER) of GaN.

PubMed

Jang, Dongsoo; Jue, Miyeon; Kim, Donghoi; Kim, Hwa Seob; Lee, Hyunkyu; Kim, Chinkyo

2018-03-07

On an SiO 2 -patterned c-plane sapphire substrate, GaN domains were grown with their polarity controlled in accordance with the pattern. While N-polar GaN was grown on hexagonally arranged circular openings, Ga-polar GaN was laterally overgrown on mask regions due to polarity inversion occurring at the boundary of the circular openings. After etching of N-polar GaN on the circular openings by H 3 PO 4 , this template was coated with 40-nm Si by sputtering and was slightly etched by KOH. After slight etching, a thin layer of Si left on the circular openings of sapphire,but not on GaN, was oxidized during thermal annealing and served as a dielectric mask during subsequent regrowth. Thus, the subsequent growth of GaN was made only on the existing Ga-polar GaN domains, not on the circular openings of the sapphire substrate. Transmission electron microscopy analysis revealed no sign of threading dislocations in this film. This approach may help fabricating an unholed and merged GaN film physically attached to but epitaxially separated from the SiO 2 -patterned sapphire.

Influence of the doping level on the porosity of silicon nanowires prepared by metal-assisted chemical etching

NASA Astrophysics Data System (ADS)

Geyer, Nadine; Wollschläger, Nicole; Fuhrmann, Bodo; Tonkikh, Alexander; Berger, Andreas; Werner, Peter; Jungmann, Marco; Krause-Rehberg, Reinhard; Leipner, Hartmut S.

2015-06-01

A systematic method to control the porosity of silicon nanowires is presented. This method is based on metal-assisted chemical etching (MACE) and takes advantage of an HF/H2O2 etching solution and a silver catalyst in the form of a thin patterned film deposited on a doped silicon wafer. It is found that the porosity of the etched nanowires can be controlled by the doping level of the wafer. For low doping concentrations, the wires are primarily crystalline and surrounded by only a very thin layer of porous silicon (pSi) layer, while for highly doped silicon, they are porous in their entire volume. We performed a series of controlled experiments to conclude that there exists a well-defined critical doping concentration separating the crystalline and porous regimes. Furthermore, transmission electron microscopy investigations showed that the pSi has also a crystalline morphology on a length scale smaller than the pore size, determined from positron annihilation lifetime spectroscopy to be mesoscopic. Based on the experimental evidence, we devise a theoretical model of the pSi formation during MACE and apply it for better control of the nanowire morphology.

Effects of wet etch processing on laser-induced damage of fused silica surfaces

DOE Office of Scientific and Technical Information (OSTI.GOV)

Battersby, C.L.; Kozlowski, M.R.; Sheehan, L.M.

1998-12-22

Laser-induced damage of transparent fused silica optical components by 355 nm illumination occurs primarily at surface defects produced during the grinding and polishing processes. These defects can either be surface defects or sub-surface damage.Wet etch processing in a buffered hydrogen fluoride (HF) solution has been examined as a tool for characterizing such defects. A study was conducted to understand the effects of etch depth on the damage threshold of fused silica substrates. The study used a 355 nm, 7.5 ns, 10 Hz Nd:YAG laser to damage test fused silica optics through various wet etch processing steps. Inspection of the surfacemore » quality was performed with Nomarski microscopy and Total Internal Reflection Microscopy. The damage test data and inspection results were correlated with polishing process specifics. The results show that a wet etch exposes subsurface damage while maintaining or improving the laser damage performance. The benefits of a wet etch must be evaluated for each polishing process.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Danno, Katsunori; Kimoto, Tsunenobu

The authors have investigated deep levels in as-grown and electron-irradiated p-type 4H-SiC epilayers by deep level transient spectroscopy. In as-grown epilayers, the D center and four deep levels are observed. In p-type 4H-SiC, reactive ion etching followed by thermal treatment (at 1150 degree sign C) induces the HK0 (E{sub V}+0.79 eV) and HK2 (E{sub V}+0.84 eV) centers. By the electron irradiation, two deep levels at 0.98 eV (EP1) and 1.44 eV (EP2) are observed in all the samples irradiated at 116-400 keV, while two additional deep levels (EP3 and EP4) are observed only in the samples irradiated at 400 keV.more » After annealing at 950 degree sign C, these centers are annealed out, and the HK4 (E{sub V}+1.44 eV) concentration is increased. By the electron irradiation at more than 160 keV followed by annealing at 950 degree sign C, three deep levels are always observed at 0.30 eV (UK1), 0.58 eV (UK2), and 1.44 eV (HK4). These centers may be defect complexes including carbon displacement-related defects. All the centers except for the D center are reduced to below the detection limit (1-3x10{sup 11} cm{sup -3}) by annealing at 1550 degree sign C for 30 min.« less

A study of laser surface treatment in bonded repair of composite aircraft structures.

PubMed

Li, Shaolong; Sun, Ting; Liu, Chang; Yang, Wenfeng; Tang, Qingru

2018-03-01

Surface pre-treatment is one of the key processes in bonded repair of aircraft carbon fibre reinforced polymer composites. This paper investigates the surface modification of physical and chemical properties by laser ablation and conventional polish treatment techniques. Surface morphology analysed by laser scanning confocal microscopy and scanning electron microscopy showed that a laser-treated surface displayed higher roughness than that of a polish-treated specimen. The laser-treated laminate exhibited more functional groups in the form of O 1 s/C 1 s atomic ratio of 30.89% for laser-treated and 20.14% for polish-treated as evidenced by X-ray photoelectron spectroscopy observation. Contact angle goniometry demonstrated that laser treatment can provide increased surface free energy and wettability. In the light of mechanical interlocking, molecular bonding and thermodynamics theories on adhesion, laser etching process displayed enhanced bonding performance relative to the polishing surface treatment. These properties resulted in an increased single lap shear strength and a cohesive failure mode for laser etching while an adhesive failure mode occurred in polish-treated specimen.

Self-assembled nanoparticle arrays as nanomasks for pattern transfer

NASA Astrophysics Data System (ADS)

Sachan, M.; Bonnoit, C.; Hogg, C.; Evarts, E.; Bain, J. A.; Majetich, S. A.; Park, J.-H.; Zhu, J.-G.

2008-07-01

Argon ion milling was used to transfer the pattern of sparse 12 nm iron oxide nanoparticles into underlying thin films of Pt and magnetic tunnel junction stacks and quantify their etching rates and morphological evolution. Under typical milling conditions, Pt milled at 10 nm min-1, while the isolated particles of iron oxide used for the mask milled at 5 nm min-1. Dilute dispersions of nanoparticles were used to produce the sparse nanomasks, and high resolution scanning electron microscopy (SEM) and atomic force microscopy were used to monitor the evolution of etched structures as a function of milling time. SEM measurements indicate an apparent 20% increase in feature diameter before the features began to diminish under additional milling, suggesting redeposition as a limiting feature in the milling of dense arrays. Simulations of the milling process in nanoparticle arrays that include redeposition are consistent with this observation. These simulations predict that an edge-to-edge spacing of 3 nm in a dense array is feasible, but that redeposition reduces the final structure aspect ratio from that of the masking array by as much as a factor of two.

A study of laser surface treatment in bonded repair of composite aircraft structures

NASA Astrophysics Data System (ADS)

Li, Shaolong; Sun, Ting; Liu, Chang; Yang, Wenfeng; Tang, Qingru

2018-03-01

Surface pre-treatment is one of the key processes in bonded repair of aircraft carbon fibre reinforced polymer composites. This paper investigates the surface modification of physical and chemical properties by laser ablation and conventional polish treatment techniques. Surface morphology analysed by laser scanning confocal microscopy and scanning electron microscopy showed that a laser-treated surface displayed higher roughness than that of a polish-treated specimen. The laser-treated laminate exhibited more functional groups in the form of O 1 s/C 1 s atomic ratio of 30.89% for laser-treated and 20.14% for polish-treated as evidenced by X-ray photoelectron spectroscopy observation. Contact angle goniometry demonstrated that laser treatment can provide increased surface free energy and wettability. In the light of mechanical interlocking, molecular bonding and thermodynamics theories on adhesion, laser etching process displayed enhanced bonding performance relative to the polishing surface treatment. These properties resulted in an increased single lap shear strength and a cohesive failure mode for laser etching while an adhesive failure mode occurred in polish-treated specimen.

A study of laser surface treatment in bonded repair of composite aircraft structures

PubMed Central

Sun, Ting; Liu, Chang; Yang, Wenfeng; Tang, Qingru

2018-01-01

Surface pre-treatment is one of the key processes in bonded repair of aircraft carbon fibre reinforced polymer composites. This paper investigates the surface modification of physical and chemical properties by laser ablation and conventional polish treatment techniques. Surface morphology analysed by laser scanning confocal microscopy and scanning electron microscopy showed that a laser-treated surface displayed higher roughness than that of a polish-treated specimen. The laser-treated laminate exhibited more functional groups in the form of O 1 s/C 1 s atomic ratio of 30.89% for laser-treated and 20.14% for polish-treated as evidenced by X-ray photoelectron spectroscopy observation. Contact angle goniometry demonstrated that laser treatment can provide increased surface free energy and wettability. In the light of mechanical interlocking, molecular bonding and thermodynamics theories on adhesion, laser etching process displayed enhanced bonding performance relative to the polishing surface treatment. These properties resulted in an increased single lap shear strength and a cohesive failure mode for laser etching while an adhesive failure mode occurred in polish-treated specimen. PMID:29657748

Electrodeposited Ni nanowires-track etched P.E.T. composites as selective solar absorbers

NASA Astrophysics Data System (ADS)

Lukhwa, R.; Sone, B.; Kotsedi, L.; Madjoe, R.; Maaza, M.

2018-05-01

This contribution reports on the structural, optical and morphological properties of nanostructured flexible solar-thermal selective absorber composites for low temperature applications. The candidate material in the system is consisting of electrodeposited nickel nano-cylinders embedded in track-etched polyethylene terephthalate (PET) host membrane of pore sizes ranging between 0.3-0.8µm supported by conductive nickel thin film of about 0.5µm. PET were irradiated with 11MeV/u high charged xenon (Xe) ions at normal incidence. The tubular and metallic structure of the nickel nano-cylinders within the insulator polymeric host forms a typical ceramic-metal nano-composite "Cermet". The produced material was characterized by the following techniques: X-ray diffraction (XRD) for structural characterization to determine preferred crystallographic structure, and grain size of the materials; Scanning electron microscopy (SEM) to determine surface morphology, particle size, and visual imaging of distribution of structures on the surface of the substrate; Atomic force microscopy (AFM) to characterize surface roughness, surface morphology, and film thickness, and UV-Vis-NIR spectrophotometer to measure the reflectance, then to determine solar absorption

Three outer arm dynein heavy chains of Chlamydomonas reinhardtii operate in a coordinated fashion both in vitro and in vivo.

PubMed

Takazaki, Hiroko; Liu, Zhongmei; Jin, Mingyue; Kamiya, Ritsu; Yasunaga, Takuo

2010-07-01

Outer arm dynein (OAD) in cilia and flagella contains two to three nonidentical heavy chains (HCs) that possess motor activity. In Chlamydomonas, flagellar OAD contains three HCs, alpha-, beta-, and gamma-HCs, each appearing to have a distinct role. To determine the precise molecular mechanism of their function, cross-sectional electron micrographs of wild-type and single HC-disruption mutants were compared and statistically analyzed. While the alpha-HC mutant displayed an OAD of lower density, which was attributed to a lack of alpha-HC, the OAD of beta- and gamma-HC mutants not only lacked the corresponding HC, but was also significantly affected in its structure, particularly with respect to the localization of alpha-HC. The lack of beta-HC induced mislocalization of alpha-HC, while a disruption of the gamma-HC gene resulted in the synchronized movement of alpha-HC and beta-HC in the manners for stacking. Interestingly, using cryo-electron microscopy, purified OADs were typically observed consisting of two stacked heads and an independent single head, which presumably corresponded to gamma-HC. This conformation is different from previous reports in which the three HCs displayed a stacked form in flagella observed by cryo-electron tomography and a bouquet structure on mica in deep-etch replica images. These results suggest that gamma-HC supports the tight stacking arrangement of inter or intra alpha-/beta-HC to facilitate the proper functioning of OAD. 2010 Wiley-Liss, Inc.

Deep-etch visualization of proteins involved in clathrin assembly

PubMed Central

1988-01-01

Assembly proteins were extracted from bovine brain clathrin-coated vesicles with 0.5 M Tris and purified by clathrin-Sepharose affinity chromatography, then adsorbed to mica and examined by freeze-etch electron microscopy. The fraction possessing maximal ability to promote clathrin polymerization, termed AP-2, was found to be a tripartite structure composed of a relatively large central mass flanked by two smaller mirror-symmetric appendages. Elastase treatment quantitatively removed the appendages and clipped 35 kD from the molecule's major approximately 105-kD polypeptides, indicating that the appendages are made from portions of these polypeptides. The remaining central masses no longer promote clathrin polymerization, suggesting that the appendages are somehow involved in the clathrin assembly reaction. The central masses are themselves relatively compact and brick-shaped, and are sufficiently large to contain two copies of the molecule's other major polypeptides (16- and 50-kD), as well as two copies of the approximately 70-kD protease-resistant portions of the major approximately 105-kD polypeptides. Thus the native molecule seems to be a dimeric, bilaterally symmetrical entity. Direct visualization of AP-2 binding to clathrin was accomplished by preparing mixtures of the two molecules in buffers that marginally inhibit AP-2 aggregation and cage assembly. This revealed numerous examples of AP-2 molecules binding to the so-called terminal domains of clathrin triskelions, consistent with earlier electron microscopic evidence that in fully assembled cages, the AP's attach centrally to inwardly-directed terminal domains of the clathrin molecule. This would place AP-2s between the clathrin coat and the enclosed membrane in whole coated vesicles. AP-2s linked to the membrane were also visualized by enzymatically removing the clathrin from brain coated vesicles, using purified 70 kD, uncoating ATPase plus ATP. This revealed several brick-shaped molecules attached to the vesicle membrane by short stalks. The exact stoichiometry of APs to clathrin in such vesicles, before and after uncoating, remains to be determined. PMID:3417785

Chemically etched fiber tips for near-field optical microscopy: a process for smoother tips.

PubMed

Lambelet, P; Sayah, A; Pfeffer, M; Philipona, C; Marquis-Weible, F

1998-11-01

An improved method for producing fiber tips for scanning near-field optical microscopy is presented. The improvement consists of chemically etching quartz optical fibers through their acrylate jacket. This new method is compared with the previous one in which bare fibers were etched. With the new process the meniscus formed by the acid along the fiber does not move during etching, leading to a much smoother surface of the tip cone. Subsequent metallization is thus improved, resulting in better coverage of the tip with an aluminum opaque layer. Our results show that leakage can be avoided along the cone, and light transmission through the tip is spatially limited to an optical aperture of a 100-nm dimension.

Visualization of pores (export sites) correlated with cellulose production in the envelope of the gram-negative bacterium Acetobacter xylinum.

PubMed

Zaar, K

1979-03-01

The Gram-negative bacterium Acetobacter xylinum assembles a cellulse ribbon composed of a number of microfibrils in the longitudinal axis of its envelope. The zone of ribbon assembly was investigated by freeze-etch electron microscopy. Freeze-etching revealed, beneath the cellulose ribbons, a linear array of pores on the lipopolysaccharide membrane. These pores have a rim diameter of 120--150 A and a central hole or deepening of approximately 35 A. The axes of pore arrays closely coincide with linear arrays of 100 A particles on the E- and P-faces of the fractured lipopolysaccharide membranes. Pores and particles in the lipopolysaccharide membrane are probably congruent. The pores are hypothesized to be the export sites (penetration sites) for cellulose.

Micromirror arrays to assess luminescent nano-objects.

PubMed

Kawakami, Yoichi; Kanai, Akinobu; Kaneta, Akio; Funato, Mitsuru; Kikuchi, Akihiko; Kishino, Katsumi

2011-05-01

We propose an array of submicrometer mirrors to assess luminescent nano-objects. Micromirror arrays (MMAs) are fabricated on Si (001) wafers via selectively doping Ga using the focused ion beam technique to form p-type etch stop regions, subsequent anisotropic chemical etching, and Al deposition. MMAs provide two benefits: reflection of luminescence from nano-objects within MMAs toward the Si (001) surface normal and nano-object labeling. The former increases the probability of optics collecting luminescence and is demonstrated by simulations based on the ray-tracing and finite-difference time-domain methods as well as by experiments. The latter enables different measurements to be repeatedly performed on a single nano-object located at a certain micromirror. For example, a single InGaN∕GaN nanocolumn is assessed by scanning electron microscopy and microphotoluminescence spectroscopy.

Rubbing time and bonding performance of one-step adhesives to primary enamel and dentin.

PubMed

Botelho, Maria Paula Jacobucci; Isolan, Cristina Pereira; Schwantz, Júlia Kaster; Lopes, Murilo Baena; Moraes, Rafael Ratto de

2017-01-01

This study investigated whether increasing the concentration of acidic monomers in one-step adhesives would allow reducing their application time without interfering with the bonding ability to primary enamel and dentin. Experimental one-step self-etch adhesives were formulated with 5 wt% (AD5), 20 wt% (AD20), or 35 wt% (AD35) acidic monomer. The adhesives were applied using rubbing motion for 5, 10, or 20 s. Bond strengths to primary enamel and dentin were tested under shear stress. A commercial etch-and-rinse adhesive (Single Bond 2; 3M ESPE) served as reference. Scanning electron microscopy was used to observe the morphology of bonded interfaces. Data were analysed at p<0.05. In enamel, AD35 had higher bond strength when rubbed for at least 10 s, while application for 5 s generated lower bond strength. In dentin, increased acidic monomer improved bonding only for 20 s rubbing time. The etch-and-rinse adhesive yielded higher bond strength to enamel and similar bonding to dentin as compared with the self-etch adhesives. The adhesive layer was thicker and more irregular for the etch-and-rinse material, with no appreciable differences among the self-etch systems. Overall, increasing the acidic monomer concentration only led to an increase in bond strength to enamel when the rubbing time was at least 10 s. In dentin, despite the increase in bond strength with longer rubbing times, the results favoured the experimental adhesives compared to the conventional adhesive. Reduced rubbing time of self-etch adhesives should be avoided in the clinical setup.

Effect of carbonated water manufactured by a soda carbonator on etched or sealed enamel

PubMed Central

Ryu, Hyo-kyung; Kim, Yong-do; Heo, Sung-su

2018-01-01

Objective The purpose of this study was to determine the effects of carbonated water on etched or sealed enamel according to the carbonation level and the presence of calcium ions. Methods Carbonated water with different carbonation levels was manufactured by a soda carbonator. Seventy-five premolar teeth were randomly divided into a control group and 4 experimental groups in accordance with the carbonation level and the presence of calcium ions in the test solutions. After specimen preparation of the Unexposed, Etched, and Sealed enamel subgroups, all the specimens were submerged in each test solution for 15 minutes three times a day during 7 days. Microhardness tests on the Unexposed and Etched enamel subgroups were performed with 10 specimens from each group. Scanning electron microscopy (SEM) tests on the Unexposed, Etched, and Sealed enamel subgroups were performed with 5 specimens from each group. Microhardness changes in different groups were statistically compared using paired t-tests, the Wilcoxon signed rank test, and the Kruskal-Wallis test. Results The microhardness changes were significantly different between the groups (p = 0.000). The microhardness changes in all experimental groups except Group 3 (low-level carbonated water with calcium ions) were significantly greater than those in the Control group. SEM showed that etched areas of the specimen were affected by carbonated water and the magnitude of destruction varied between groups. Adhesive material was partially removed in groups exposed to carbonated water. Conclusions Carbonated water has negative effects on etched or sealed enamel, resulting in decreased microhardness and removal of the adhesive material. PMID:29291188

Comparing the shear bond strength of direct and indirect composite inlays in relation to different surface conditioning and curing techniques

PubMed Central

Zorba, Yahya Orcun; Ilday, Nurcan Ozakar; Bayındır, Yusuf Ziya; Demirbuga, Sezer

2013-01-01

Objective: The aim of this study was to test the null hypothesis that different surface conditioning (etch and rinse and self-etch) and curing techniques (light cure/dual cure) had no effect on the shear bond strength of direct and indirect composite inlays. Materials and Methods: A total of 112 extracted human molar teeth were horizontally sectioned and randomly divided into two groups according to restoration technique (direct and indirect restorations). Each group was further subdivided into seven subgroups (n = 8) according to bonding agent (etch and rinse adhesives Scotchbond multi-purpose plus, All-Bond 3, Adper Single Bond and Prime Bond NT; and self-etch adhesives Clearfil Liner Bond, Futurabond DC and G bond). Indirect composites were cemented to dentin surfaces using dual-curing luting cement. Shear bond strength of specimens was tested using a Universal Testing Machine. Two samples from each subgroup were evaluated under Scanning electron microscopy to see the failing modes. Data was analyzed using independent sample t-tests and Tukey's tests. Results: Surface conditioning and curing of bonding agents were all found to have significant effects on shear bond strength (P < 0.05) of both direct and indirect composite inlays. With direct restoration, etch and rinse systems and dual-cured bonding agents yielded higher bond strengths than indirect restoration, self-etch systems and light-cured bonding agents. Conclusions: The results of the present study indicated that direct restoration to be a more reliable method than indirect restoration. Although etch and rinse bonding systems showed higher shear bond strength to dentin than self-etch systems, both systems can be safely used for the adhesion of direct as well as indirect restorations. PMID:24932118

Comparing the shear bond strength of direct and indirect composite inlays in relation to different surface conditioning and curing techniques.

PubMed

Zorba, Yahya Orcun; Ilday, Nurcan Ozakar; Bayındır, Yusuf Ziya; Demirbuga, Sezer

2013-10-01

The aim of this study was to test the null hypothesis that different surface conditioning (etch and rinse and self-etch) and curing techniques (light cure/dual cure) had no effect on the shear bond strength of direct and indirect composite inlays. A total of 112 extracted human molar teeth were horizontally sectioned and randomly divided into two groups according to restoration technique (direct and indirect restorations). Each group was further subdivided into seven subgroups (n = 8) according to bonding agent (etch and rinse adhesives Scotchbond multi-purpose plus, All-Bond 3, Adper Single Bond and Prime Bond NT; and self-etch adhesives Clearfil Liner Bond, Futurabond DC and G bond). Indirect composites were cemented to dentin surfaces using dual-curing luting cement. Shear bond strength of specimens was tested using a Universal Testing Machine. Two samples from each subgroup were evaluated under Scanning electron microscopy to see the failing modes. Data was analyzed using independent sample t-tests and Tukey's tests. Surface conditioning and curing of bonding agents were all found to have significant effects on shear bond strength (P < 0.05) of both direct and indirect composite inlays. With direct restoration, etch and rinse systems and dual-cured bonding agents yielded higher bond strengths than indirect restoration, self-etch systems and light-cured bonding agents. The results of the present study indicated that direct restoration to be a more reliable method than indirect restoration. Although etch and rinse bonding systems showed higher shear bond strength to dentin than self-etch systems, both systems can be safely used for the adhesion of direct as well as indirect restorations.

Electroluminescence and other diagnostic techniques for the study of hot-electron effects in compound semiconductor devices

NASA Astrophysics Data System (ADS)

Zanoni, Enrico; Meneghesso, Gaudenzio; Menozzi, Roberto

2000-03-01

Hot electron in III-V FETs can be indirectly monitored by measuring the current coming out from the gate when the device is biased at high electric fields. This negative current is due to the collection of holes generated by impact ionization in the gate-to drain region. Electroluminescence represents a powerful tool in order to characterize not only hot electrons but also material properties. By using spatially resolved emission microscopy it is possible to show that the light due to cold electron/hole recombination is emitted between the gate and the source (low electric field region), while the contribution due to hot electrons is emitted between the gate and the drain (high electric field region). Deep-traps created in the device by hot carriers can be analysed by means of drain current deep level transient spectroscopy and by transconductance frequency dispersion. Cathodoluminescence, optical beam induced current, X-ray spectroscopy, electron energy loss spectroscopy in combination with a transmission electron microscopy are powerful tools in order to identify and localize surface modification following hot-electron stress tests.

The use of a 'bleach-etch-seal' deproteinization technique on MIH affected enamel.

PubMed

Gandhi, Shan; Crawford, Peter; Shellis, Peter

2012-11-01

To ascertain whether deproteinization pretreatment of molar-incisor hypomineralization (MIH) enamel affects resin sealant infiltration. Thirty one extracted MIH teeth were divided into three sections and randomly allocated into the Control (etch and FS), Treatment 1 (5% NaOCl, etched and fissure sealed), and Treatment 2 (5% NaOCl and fissure sealed with no etch) groups. Two hundred seventy nine sealant tag/enamel grade observations were recorded by scanning electron microscopy. Control and Treatment 1 were similar in their outcomes, and Treatment 2 was markedly different. There was no statistical evidence to suggest that there was any difference between Treatment 1 and the Control Treatment (95% CI, 0.52, 1.51; P = 0.6). There was a marked difference between Treatment 2 and the Control Treatment (95% CI, 0.07, 0.25; P < 0.001). All treatments also demonstrated a high-predicted probability of obtaining 'poor' sealant tags (Control = 47%, Treatment 1 = 49%, and Treatment 2 = 40%). The findings suggest that there was no significant difference in the tag quality between the conventional technique (Control) and the 'bleach-etch-seal' technique (Treatment 1). There was no benefit in pre-treating with NaOCl alone (without etch) before sealing. This research also showed that there was a high-predicted probability of obtaining 'poor' sealant tags in MIH enamel, regardless of which of the three treatments was used. © 2012 The Authors. International Journal of Paediatric Dentistry © 2012 BSPD, IAPD and Blackwell Publishing Ltd.

Optical properties of template synthesized nanowalled ZnS microtubules

NASA Astrophysics Data System (ADS)

Kumar, Rajesh; Chakarvarti, S. K.

2007-12-01

Electrodeposition is a versatile technique combining low processing cost with ambient conditions that can be used to prepare metallic, polymeric and semiconducting nano/micro structures. In the present work, track-etch membranes (TEMs) of makrofol (KG) have been used as templates for synthesis of ZnS nanowalled microtubules using electrodeposition technique. The morphology of the microtubules was characterized by scanning electron microscopy. Size effects on the band gap of tubules have also been studied by UV-visible spectrophotometer.

Preparation of titanium dioxide films on etched aluminum foil by vacuum infiltration and anodizing

NASA Astrophysics Data System (ADS)

Xiang, Lian; Park, Sang-Shik

2016-12-01

Al2O3-TiO2 (Al-Ti) composite oxide films are a promising dielectric material for future use in capacitors. In this study, TiO2 films were prepared on etched Al foils by vacuum infiltration. TiO2 films prepared using a sol-gel process were annealed at various temperatures (450, 500, and 550 °C) for different time durations (10, 30, and 60 min) for 4 cycles, and then anodized at 100 V. The specimens were characterized using X-ray diffraction, field emission scanning electron microscopy, and field emission transmission electron microscopy. The results show that the tunnels of the specimens feature a multi-layer structure consisting of an Al2O3 outer layer, an Al-Ti composite oxide middle layer, and an aluminum hydrate inner layer. The electrical properties of the specimens, such as the withstanding voltage and specific capacitance, were also measured. Compared to specimens without TiO2 coating, the specific capacitances of the TiO2-coated specimens are increased. The specific capacitance of the anode Al foil with TiO2 coating increased by 42% compared to that of a specimen without TiO2 coating when annealed at 550 °C for 10 min. These composite oxide films could enhance the specific capacitance of anode Al foils used in dielectric materials.

Influence of two different template removal methods on the micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres

NASA Astrophysics Data System (ADS)

Wang, Han; Jin, Tingting; Zheng, Xing; Jiang, Bo; Zhu, Chaosheng; Yuan, Xiangdong; Zheng, Jingtang; Wu, Mingbo

2016-11-01

Hollow cadmium sulfide (CdS) nanospheres of about 260 nm average diameters and about 30 nm shell thickness can be easily synthesized via a sonochemical process, in which polystyrene (PS) nanoparticles were employed as templates. In order to remove the PS templates, both etching and calcination were applied in this paper. The influence of the two different template removal methods on the surface micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres was carefully performed a comparative study. Results of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray, FT-IR, thermogravimetric analysis, Brunauer-Emmett-Teller, diffused reflectance spectra, and decolorization experiments showed that the different template removal methods exhibited a significant influence on the surface micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres. The CdS hollow nanospheres as-prepared by etching had pure cubic sphalerite structure, higher -OH content, less defects and exhibited good photocatalytic activity for rhodamine-B, Methylene Blue and methyl orange under UV-vis light irradiation. However, CdS hollow nanospheres obtained by calcination with a hexagonal crystal structure, less -OH content, more defects have shown worse photocatalytic activity. This indicated that surface micromorphology and crystalline phase were mainly factors influencing photocatalytic activity of hollow CdS nanospheres.

Cell adhesion on nanotextured slippery superhydrophobic substrates.

PubMed

Di Mundo, Rosa; Nardulli, Marina; Milella, Antonella; Favia, Pietro; d'Agostino, Riccardo; Gristina, Roberto

2011-04-19

In this work, the response of Saos2 cells to polymeric surfaces with different roughness/density of nanometric dots produced by a tailored plasma-etching process has been studied. Topographical features have been evaluated by atomic force microscopy, while wetting behavior, in terms of water-surface adhesion energy, has been evaluated by measurements of drop sliding angle. Saos2 cytocompatibility has been investigated by scanning electron microscopy, fluorescent microscopy, and optical microscopy. The similarity in outer chemical composition has allowed isolation of the impact of the topographical features on cellular behavior. The results indicate that Saos2 cells respond differently to surfaces with different nanoscale topographical features, clearly showing a certain inhibition in cell adhesion when the nanoscale is particularly small. This effect appears to be attenuated in surfaces with relatively bigger nanofeatures, though these express a more pronounced slippery/dry wetting character. © 2011 American Chemical Society

Effect of Phosphoric Acid Pre-etching on Fatigue Limits of Self-etching Adhesives.

PubMed

Takamizawa, T; Barkmeier, W W; Tsujimoto, A; Scheidel, D D; Erickson, R L; Latta, M A; Miyazaki, M

2015-01-01

The purpose of this study was to use shear bond strength (SBS) and shear fatigue limit (SFL) testing to determine the effect of phosphoric acid pre-etching of enamel and dentin prior to application of self-etch adhesives for bonding resin composite to these substrates. Three self-etch adhesives--1) G- ænial Bond (GC Corporation, Tokyo, Japan); 2) OptiBond XTR (Kerr Corp, Orange, CA, USA); and 3) Scotchbond Universal (3M ESPE Dental Products, St Paul, MN, USA)--were used to bond Z100 Restorative resin composite to enamel and dentin surfaces. A stainless-steel metal ring with an inner diameter of 2.4 mm was used to bond the resin composite to flat-ground (4000 grit) tooth surfaces for determination of both SBS and SFL. Fifteen specimens each were used to determine initial SBS to human enamel/dentin, with and without pre-etching with a 35% phosphoric acid (Ultra-Etch, Ultradent Products Inc, South Jordan, UT, USA) for 15 seconds prior to the application of the adhesives. A staircase method of fatigue testing (25 specimens for each test) was then used to determine the SFL of resin composite bonded to enamel/dentin using a frequency of 10 Hz for 50,000 cycles or until failure occurred. A two-way analysis of variance and Tukey post hoc test were used for analysis of SBS data, and a modified t-test with Bonferroni correction was used for the SFL data. Scanning electron microscopy was used to examine the area of the bonded restorative/tooth interface. For all three adhesive systems, phosphoric acid pre-etching of enamel demonstrated significantly higher (p<0.05) SBS and SFL with pre-etching than it did without pre-etching. The SBS and SFL of dentin bonds decreased with phosphoric acid pre-etching. The SBS and SFL of bonds using phosphoric acid prior to application of self-etching adhesives clearly demonstrated different tendencies between enamel and dentin. The effect of using phosphoric acid, prior to the application of the self-etching adhesives, on SBS and SFL was dependent on the adhesive material and tooth substrate and should be carefully considered in clinical situations.

Influence of Etching Mode on Enamel Bond Durability of Universal Adhesive Systems.

PubMed

Suzuki, T; Takamizawa, T; Barkmeier, W W; Tsujimoto, A; Endo, H; Erickson, R L; Latta, M A; Miyazaki, M

2016-01-01

The purpose of this study was to determine the enamel bond durability of three universal adhesives in different etching modes through fatigue testing. The three universal adhesives used were Scotchbond Universal, Prime&Bond Elect universal dental adhesive, and All-Bond Universal light-cured dental adhesive. A single-step self-etch adhesive, Clearfil S 3 Bond Plus was used as a control. The shear bond strength (SBS) and shear fatigue strength (SFS) to human enamel were evaluated in total-etch mode and self-etch mode. A stainless steel metal ring with an internal diameter of 2.4 mm was used to bond the resin composite to the flat-ground (4000-grit) tooth surfaces for determination of both SBS and SFS. For each enamel surface treatment, 15 specimens were prepared for SBS and 30 specimens for SFS. The staircase method for fatigue testing was then used to determine the SFS of the resin composite bonded to the enamel using 10-Hz frequencies for 50,000 cycles or until failure occurred. Scanning electron microscopy was used to observe representative debonded specimen surfaces and the resin-enamel interfaces. A two-way analysis of variance and the Tukey post hoc test were used for analysis of the SBS data, whereas a modified t-test with Bonferroni correction was used for the SFS data. All adhesives in total-etch mode showed significantly higher SBS and SFS values than those in self-etch mode. Although All-Bond Universal in self-etch mode showed a significantly lower SBS value than the other adhesives, there was no significant difference in SFS values among the adhesives in this mode. All adhesives showed higher SFS:SBS ratios in total-etch mode than in self-etch mode. With regard to the adhesive systems used in this study, universal adhesives showed higher enamel bond strengths in total-etch mode. Although the influence of different etching modes on the enamel-bonding performance of universal adhesives was found to be dependent on the adhesive material, total-etch mode effectively increased the enamel bond strength and durability, as measured by fatigue testing.

No-waiting dentine self-etch concept-Merit or hype.

PubMed

Huang, Xue-Qing; Pucci, César R; Luo, Tao; Breschi, Lorenzo; Pashley, David H; Niu, Li-Na; Tay, Franklin R

2017-07-01

A recently-launched universal adhesive, G-Premio Bond, provides clinicians with the alternative to use the self-etch technique for bonding to dentine without waiting for the adhesive to interact with the bonding substrate (no-waiting self-etch; Japanese brochure), or after leaving the adhesive undisturbed for 10s (10-s self-etch; international brochure). The present study was performed to examine in vitro performance of this new universal adhesive bonded to human coronal dentine using the two alternative self-etch modes. One hundred and ten specimens were bonded using two self-etch application modes and examined with or without thermomechanical cycling (10,000 thermal cycles and 240,000 mechanical cycles) to simulate one year of intraoral functioning. The bonded specimens were sectioned for microtensile bond testing, ultrastructural and nanoleakage examination using transmission electron microscopy. Changes in the composition of mineralised dentine after adhesive application were examined using Fourier transform infrared spectroscopy. Both reduced application time and thermomechanical cycling resulted in significantly lower bond strengths, thinner hybrid layers, and significantly more extensive nanoleakage after thermomechanical cycling. Using the conventional 10-s application time improved bonding performance when compared with the no-waiting self-etch technique. Nevertheless, nanoleakage was generally extensive under all testing parameters employed for examining the adhesive. Although sufficient bond strength to dentine may be achieved using the present universal adhesive in the no-waiting self-etch mode that does not require clinicians to wait prior to polymerisation of the adhesive, this self-etch concept requires further technological refinement before it can be recommended as a clinical technique. Although the surge for cutting application time to increase user friendliness remains the most frequently sought conduit for advancement of dentine bonding technology, the use of the present universal adhesive in the no-waiting self-etch mode may not represent the best use of the adhesive. Published by Elsevier Ltd.

Layer Number and Stacking Order Imaging of Few-layer Graphenes by Transmission Electron Microscopy

NASA Astrophysics Data System (ADS)

Ping, Jinglei; Fuhrer, Michael

2012-02-01

A method using transmission electron microscopy (TEM) selected area electron diffraction (SAED) patterns and dark field (DF) images is developed to identify graphene layer number and stacking order by comparing intensity ratios of SAED spots with theory. Graphene samples are synthesized by ambient pressure chemical vapor depostion and then etched by hydrogen in high temperature to produce samples with crystalline stacking but varying layer number on the nanometer scale. Combined DF images from first- and second-order diffraction spots are used to produce images with layer-number and stacking-order contrast with few-nanometer resolution. This method is proved to be accurate enough for quantative stacking-order-identification of graphenes up to at least four layers. This work was partially supported by Science of Precision Multifunctional Nanostructures for Elecrical Energy Storage, an Energy Frontier Research Center funded by the U.S. DOE, Office of Science, Office of Basic Energy Sciences under Award Number DESC0001160.

Functionalised polyurethane for efficient laser micromachining

NASA Astrophysics Data System (ADS)

Brodie, G. W. J.; Kang, H.; MacMillan, F. J.; Jin, J.; Simpson, M. C.

2017-02-01

Pulsed laser ablation is a valuable tool that offers a much cleaner and more flexible etching process than conventional lithographic techniques. Although much research has been undertaken on commercially available polymers, many challenges still remain, including contamination by debris on the surface, a rough etched appearance and high ablation thresholds. Functionalizing polymers with a photosensitive group is a novel way and effective way to improve the efficiency of laser micromachining. In this study, several polyurethane films grafted with different concentrations of the chromophore anthracene have been synthesized which are specifically designed for 248 nm KrF excimer laser ablation. A series of lines etched with a changing number of pulses and fluences by the nanosecond laser were applied to each polyurethane film. The resultant ablation behaviours were studied through optical interference tomography and Scanning Electron Microscopy. The anthracene grafted polyurethanes showed a vast improvement in both edge quality and the presence of debris compared with the unmodified polyurethane. Under the same laser fluence and number of pulses the spots etched in the anthracene contained polyurethane show sharp depth profiles and smooth surfaces, whereas the spots etched in polyurethane without anthracene group grafted present rough cavities with debris according to the SEM images. The addition of a small amount of anthracene (1.47%) shows a reduction in ablation threshold from unmodified polyurethane showing that the desired effect can be achieved with very little modification to the polymer.

Fiber post etching with hydrogen peroxide: effect of concentration and application time.

PubMed

de Sousa Menezes, Murilo; Queiroz, Ellyne Cavalcanti; Soares, Paulo Vinícius; Faria-e-Silva, André Luis; Soares, Carlos José; Martins, Luis Roberto Marcondes

2011-03-01

Etching is necessary to expose the fibers and enable both mechanical and chemical bonding of the resin core to the fiber post. This study evaluated the effect of concentration and application time of hydrogen peroxide on the surface topography and bond strength of glass fiber posts to resin cores. Fiber posts were etched with 24% or 50% hydrogen peroxide for 1, 5, or 10 min (n = 10). Posts without any treatment were used as a control. After etching, the posts were silanated and adhesive resin was applied. The posts were positioned into a mold to allow a self-cured resin core to be inserted. The post/resin assembly was serially sectioned into five beams that were subjected to a tensile bond strength test. Data were subjected to two-way ANOVA and Tukey test (α = 0.05). The surface topography was analyzed using scanning electronic microscopy. Non-etched post presents a relatively smooth surface without fiber exposure. Application of hydrogen peroxide increased the surface roughness and exposed the fibers. All experimental conditions yielded similar bond strength values that were higher than those obtained in the control group. Both 24% and 50% hydrogen peroxide exposure increased the bond strength of resin to the posts, irrespective of the application time. Copyright © 2011 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

NCI Scientists Get Deep Look at CRISPR Complex Through Deep Freeze | Poster

Cancer.gov

To get a closer look at one CRISPR complex, researchers from NCI’s Center for Cancer Research and their collaborators recently put it “on ice” with cryo-electron microscopy, creating highly detailed images that show its biological structures in multiple states at a molecular level.

Defect-Enabled Electrical Current Leakage in Ultraviolet Light-Emitting Diodes

DOE PAGES

Moseley, Michael William; Allerman, Andrew A.; Crawford, Mary H.; ...

2015-04-13

The AlGaN materials system offers a tunable, ultra-wide bandgap that is exceptionally useful for high-power electronics and deep ultraviolet optoelectronics. Moseley et al. (pp. 723–726) investigate a structural defect known as an open-core threading dislocation or ''nanopipe'' that is particularly detrimental to devices that employ these materials. Furthermore, an AlGaN thin film was synthesized using metal-organic chemical-vapor deposition. Electrical current leakage is detected at a discrete point using a conductive atomic-force microscope (CAFM). However, no physical feature or abnormality at this location was visible by an optical microscope. The AlGaN thin film was then etched in hot phosphoric acid, andmore » the same location that was previously analyzed was revisited with the CAFM. The point that previously exhibited electrical current leakage had been decorated with a 1.1 μm wide hexagonal pit, which identified the site of electrical current leakage as a nanopipe and allows these defects to be easily observed by optical microscopy. Moreover, with this nanopipe identification and quantification strategy, the authors were able to correlate decreasing ultraviolet light-emitting diode optical output power with increasing nanopipe density.« less

Plasma etching of superconducting Niobium tips for scanning tunneling microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roychowdhury, A.; Center for Nanophysics and Advanced Materials, Department of Physics, University of Maryland, College Park, Maryland 20742; Dana, R.

We have developed a reproducible technique for the fabrication of sharp superconducting Nb tips for scanning tunneling microscopy (STM) and scanning tunneling spectroscopy. Sections of Nb wire with 250 μm diameter are dry etched in an SF₆ plasma in a Reactive Ion Etcher. The gas pressure, etching time, and applied power are chosen to control the ratio of isotropic to anisotropic etch rates and produce the desired tip shape. The resulting tips are atomically sharp, with radii of less than 100 nm, mechanically stable, and superconducting. They generate good STM images and spectroscopy on single crystal samples of Au(111), Au(100),more » and Nb(100), as well as a doped topological insulator Bi₂Se₃ at temperatures ranging from 30 mK to 9 K.« less

Effect of crystallographic orientation on the anodic formation of nanoscale pores/tubes in TiO 2 films

NASA Astrophysics Data System (ADS)

Kalantar-zadeh, K.; Sadek, A. Z.; Zheng, H.; Partridge, J. G.; McCulloch, D. G.; Li, Y. X.; Yu, X. F.; Wlodarski, W.

2009-10-01

Self-organized nanopores and nanotubes have been produced in thin films of titanium (Ti) prepared using filtered cathodic vacuum arc (FCVA), DC- and RF-sputter deposition systems. The anodization process was performed using a neutral electrolyte containing fluoride ions with an applied potential between 2 and 20 V (for clarity the results are only presented for 5 V). Scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD) techniques were used to characterise the films. It was found that the crystallographic orientation of the Ti films played a significant role in determining whether pores or tubes were formed during the anodic etching process.

Study of irradiation induced surface pattern and structural changes in Inconel 718 alloy

NASA Astrophysics Data System (ADS)

Wan, Hao; Si, Naichao; Zhao, Zhenjiang; Wang, Jian; Zhang, Yifei

2018-05-01

Helium ions irradiation induced surface pattern and structural changes of Inconel 718 alloy were studied with the combined utilization of atomic force microscopy (AFM), x-ray diffraction (XRD) and transmission electron microscopy (TEM). In addition, SRIM-2013 software was used to calculate the sputtering yield and detailed collision events. The result shows that, irradiation dose play an important role in altering the pattern of the surface. Enhanced irradiation aggravated the surface etching and increased the surface roughness. In ion irradiated layer, large amount of interstitials, vacancies and defect sinks were produced. Moreover, in samples with increasing dose irradiation, the dependence of interplanar spacing variation due to point defects clustering on sink density was discussed.

Effects of dextrose and lipopolysaccharide on the corrosion behavior of a Ti-6Al-4V alloy with a smooth surface or treated with double-acid-etching.

PubMed

Faverani, Leonardo P; Assunção, Wirley G; de Carvalho, Paulo Sérgio P; Yuan, Judy Chia-Chun; Sukotjo, Cortino; Mathew, Mathew T; Barao, Valentim A

2014-01-01

Diabetes and infections are associated with a high risk of implant failure. However, the effects of such conditions on the electrochemical stability of titanium materials remain unclear. This study evaluated the corrosion behavior of a Ti-6Al-4V alloy, with a smooth surface or conditioned by double-acid-etching, in simulated body fluid with different concentrations of dextrose and lipopolysaccharide. For the electrochemical assay, the open-circuit-potential, electrochemical impedance spectroscopy, and potentiodynamic test were used. The disc surfaces were characterized by scanning electron microscopy and atomic force microscopy. Their surface roughness and Vickers microhardness were also tested. The quantitative data were analyzed by Pearson's correlation and independent t-tests (α = 0.05). In the corrosion parameters, there was a strong lipopolysaccharide correlation with the Ipass (passivation current density), Cdl (double-layer capacitance), and Rp (polarization resistance) values (p<0.05) for the Ti-6Al-4V alloy with surface treatment by double-acid-etching. The combination of dextrose and lipopolysaccharide was correlated with the Icorr (corrosion current density) and Ipass (p<0.05). The acid-treated groups showed a significant increase in Cdl values and reduced Rp values (p<0.05, t-test). According to the topography, there was an increase in surface roughness (R2 = 0.726, p<0.0001 for the smooth surface; R2 = 0.405, p = 0.036 for the double-acid-etching-treated surface). The microhardness of the smooth Ti-6Al-4V alloy decreased (p<0.05) and that of the treated Ti-6Al-4V alloy increased (p<0.0001). Atomic force microscopy showed changes in the microstructure of the Ti-6Al-4V alloy by increasing the surface thickness mainly in the group associated with dextrose and lipopolysaccharide. The combination of dextrose and lipopolysaccharide affected the corrosion behavior of the Ti-6Al-4V alloy surface treated with double-acid-etching. However, no dose-response corrosion behavior could be observed. These results suggest a greater susceptibility to corrosion of titanium implants in diabetic patients with associated infections.

Effects of Dextrose and Lipopolysaccharide on the Corrosion Behavior of a Ti-6Al-4V Alloy with a Smooth Surface or Treated with Double-Acid-Etching

PubMed Central

Faverani, Leonardo P.; Assunção, Wirley G.; de Carvalho, Paulo Sérgio P.; Yuan, Judy Chia-Chun; Sukotjo, Cortino; Mathew, Mathew T.; Barao, Valentim A.

2014-01-01

Diabetes and infections are associated with a high risk of implant failure. However, the effects of such conditions on the electrochemical stability of titanium materials remain unclear. This study evaluated the corrosion behavior of a Ti-6Al-4V alloy, with a smooth surface or conditioned by double-acid-etching, in simulated body fluid with different concentrations of dextrose and lipopolysaccharide. For the electrochemical assay, the open-circuit-potential, electrochemical impedance spectroscopy, and potentiodynamic test were used. The disc surfaces were characterized by scanning electron microscopy and atomic force microscopy. Their surface roughness and Vickers microhardness were also tested. The quantitative data were analyzed by Pearson's correlation and independent t-tests (α = 0.05). In the corrosion parameters, there was a strong lipopolysaccharide correlation with the Ipass (passivation current density), Cdl (double-layer capacitance), and Rp (polarization resistance) values (p<0.05) for the Ti-6Al-4V alloy with surface treatment by double-acid-etching. The combination of dextrose and lipopolysaccharide was correlated with the Icorr (corrosion current density) and Ipass (p<0.05). The acid-treated groups showed a significant increase in Cdl values and reduced Rp values (p<0.05, t-test). According to the topography, there was an increase in surface roughness (R2 = 0.726, p<0.0001 for the smooth surface; R2 = 0.405, p = 0.036 for the double-acid-etching-treated surface). The microhardness of the smooth Ti-6Al-4V alloy decreased (p<0.05) and that of the treated Ti-6Al-4V alloy increased (p<0.0001). Atomic force microscopy showed changes in the microstructure of the Ti-6Al-4V alloy by increasing the surface thickness mainly in the group associated with dextrose and lipopolysaccharide. The combination of dextrose and lipopolysaccharide affected the corrosion behavior of the Ti-6Al-4V alloy surface treated with double-acid-etching. However, no dose-response corrosion behavior could be observed. These results suggest a greater susceptibility to corrosion of titanium implants in diabetic patients with associated infections. PMID:24671257

InAs nanowires grown by metal-organic vapor-phase epitaxy (MOVPE) employing PS/PMMA diblock copolymer nanopatterning.

PubMed

Huang, Yinggang; Kim, Tae Wan; Xiong, Shisheng; Mawst, Luke J; Kuech, Thomas F; Nealey, Paul F; Dai, Yushuai; Wang, Zihao; Guo, Wei; Forbes, David; Hubbard, Seth M; Nesnidal, Michael

2013-01-01

Dense arrays of indium arsenide (InAs) nanowire materials have been grown by selective-area metal-organic vapor-phase epitaxy (SA-MOVPE) using polystyrene-b-poly(methyl methacrylate) (PS/PMMA) diblock copolymer (DBC) nanopatterning technique, which is a catalyst-free approach. Nanoscale openings were defined in a thin (~10 nm) SiNx layer deposited on a (111)B-oriented GaAs substrate using the DBC process and CF4 reactive ion etching (RIE), which served as a hard mask for the nanowire growth. InAs nanowires with diameters down to ~ 20 nm and micrometer-scale lengths were achieved with a density of ~ 5 × 10(10) cm(2). The nanowire structures were characterized by scanning electron microscopy and transmission electron microscopy, which indicate twin defects in a primary zincblende crystal structure and the absence of threading dislocation within the imaged regions.

Nanoepitaxy of GaAs on a Si(001) substrate using a round-hole nanopatterned SiO2 mask.

PubMed

Hsu, Chao-Wei; Chen, Yung-Feng; Su, Yan-Kuin

2012-12-14

GaAs is grown by metal-organic vapor-phase epitaxy on a 55 nm round-hole patterned Si substrate with SiO(2) as a mask. The threading dislocations, which are stacked on the lowest energy facet plane, move along the SiO(2) walls, reducing the number of dislocations. The etching pit density of GaAs on the 55 nm round-hole patterned Si substrate is about 3.3 × 10(5) cm(-2). Compared with the full width at half maximum measurement from x-ray diffraction and photoluminescence spectra of GaAs on a planar Si(001) substrate, those of GaAs on the 55 nm round-hole patterned Si substrate are reduced by 39.6 and 31.4%, respectively. The improvement in material quality is verified by transmission electron microscopy, field-emission scanning electron microscopy, Hall measurements, Raman spectroscopy, photoluminescence, and x-ray diffraction studies.

Fabrication of ordered NiO coated Si nanowire array films as electrodes for a high performance lithium ion battery.

PubMed

Qiu, M C; Yang, L W; Qi, X; Li, Jun; Zhong, J X

2010-12-01

Highly ordered NiO coated Si nanowire array films are fabricated as electrodes for a high performance lithium ion battery via depositing Ni on electroless-etched Si nanowires and subsequently annealing. The structures and morphologies of as-prepared films are characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. When the potential window versus lithium was controlled, the coated NiO can be selected to be electrochemically active to store and release Li+ ions, while highly conductive crystalline Si cores function as nothing more than a stable mechanical support and an efficient electrical conducting pathway. The hybrid nanowire array films exhibit superior cyclic stability and reversible capacity compared to that of NiO nanostructured films. Owing to the ease of large-scale fabrication and superior electrochemical performance, these hybrid nanowire array films will be promising anode materials for high performance lithium-ion batteries.

Synthesis of gold nanoflowers using deep eutectic solvent with high surface enhanced Raman scattering properties

NASA Astrophysics Data System (ADS)

Aghakhani Mahyari, Farzaneh; Tohidi, Maryam; Safavi, Afsaneh

2016-09-01

A facile, seed-less and one-pot method was developed for synthesis of gold nanoflowers with multiple tips through reduction of HAuCl4 with deep eutectic solvent at room temperature. This solvent is eco-friendly, low-cost, non-toxic and biodegradable and can act as both reducing and shape-controlling agent. In this protocol, highly branched and stable gold nanoflowers were obtained without using any capping agent. The obtained products were characterized by different techniques including, field emission scanning electron microscopy, transmission electron microscopy, x-ray diffraction and UV-vis spectroscopy. The as-prepared gold nanoflowers exhibit efficient surface-enhanced Raman scattering (SERS) properties which can be used as excellent substrates for SERS.

3D memory: etch is the new litho

NASA Astrophysics Data System (ADS)

Petti, Christopher

2018-03-01

This paper discusses the process challenges and limitations for 3D NAND processes, focusing on vertical 3D architectures. The effect of deep memory hole etches on die cost is calculated, with die cost showing a minimum at a given number of layers because of aspect-ratio dependent etch effects. Techniques to mitigate these etch effects are summarized, as are other etch issues, such as bowing and twisting. Metal replacement gate processes and their challenges are also described. Lastly, future directions of vertical 3D NAND technologies are explored.

Ion-beam-assisted etching of diamond

NASA Technical Reports Server (NTRS)

Efremow, N. N.; Geis, M. W.; Flanders, D. C.; Lincoln, G. A.; Economou, N. P.

1985-01-01

The high thermal conductivity, low RF loss, and inertness of diamond make it useful in traveling wave tubes operating in excess of 500 GHz. Such use requires the controlled etching of type IIA diamond to produce grating like structures tens of micrometers deep. Previous work on reactive ion etching with O2 gave etching rates on the order of 20 nm/min and poor etch selectivity between the masking material (Ni or Cr) and the diamond. An alternative approach which uses a Xe(+) beam and a reactive gas flux of NO2 in an ion-beam-assisted etching system is reported. An etching rate of 200 nm/min was obtained with an etching rate ratio of 20 between the diamond and an aluminum mask.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Missert, Nancy; Kotula, Paul G.; Rye, Michael

We used a focused ion beam to obtain cross-sectional specimens from both magnetic multilayer and Nb/Al-AlOx/Nb Josephson junction devices for characterization by scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX). An automated multivariate statistical analysis of the EDX spectral images produced chemically unique component images of individual layers within the multilayer structures. STEM imaging elucidated distinct variations in film morphology, interface quality, and/or etch artifacts that could be correlated to magnetic and/or electrical properties measured on the same devices.

Periodic scarred States in open quantum dots as evidence of quantum Darwinism.

PubMed

Burke, A M; Akis, R; Day, T E; Speyer, Gil; Ferry, D K; Bennett, B R

2010-04-30

Scanning gate microscopy (SGM) is used to image scar structures in an open quantum dot, which is created in an InAs quantum well by electron-beam lithography and wet etching. The scanned images demonstrate periodicities in magnetic field that correlate to those found in the conductance fluctuations. Simulations have shown that these magnetic transform images bear a strong resemblance to actual scars found in the dot that replicate through the modes in direct agreement with quantum Darwinism.

Periodic Scarred States in Open Quantum Dots as Evidence of Quantum Darwinism

NASA Astrophysics Data System (ADS)

Burke, A. M.; Akis, R.; Day, T. E.; Speyer, Gil; Ferry, D. K.; Bennett, B. R.

2010-04-01

Scanning gate microscopy (SGM) is used to image scar structures in an open quantum dot, which is created in an InAs quantum well by electron-beam lithography and wet etching. The scanned images demonstrate periodicities in magnetic field that correlate to those found in the conductance fluctuations. Simulations have shown that these magnetic transform images bear a strong resemblance to actual scars found in the dot that replicate through the modes in direct agreement with quantum Darwinism.

Etching and oxidation of InAs in planar inductively coupled plasma

NASA Astrophysics Data System (ADS)

Dultsev, F. N.; Kesler, V. G.

2009-10-01

The surface of InAs (1 1 1)A was investigated under plasmachemical etching in the gas mixture CH 4/H 2/Ar. Etching was performed using the RF (13.56 MHz) and ICP plasma with the power 30-150 and 50-300 W, respectively; gas pressure in the reactor was 3-10 mTorr. It was demonstrated that the composition of the subsurface layer less than 5 nm thick changes during plasmachemical etching. A method of deep etching of InAs involving ICP plasma and hydrocarbon based chemistry providing the conservation of the surface relief is proposed. Optimal conditions and the composition of the gas phase for plasmachemical etching ensuring acceptable etch rates were selected.

In vivo effect of a self-etching primer on dentin.

PubMed

Milia, E; Lallai, M R; García-Godoy, F

1999-08-01

To determine the ultrastructural aspects of the dentin collagen area in the cavity preparation floor produced in vivo after phosphoric acid acid-etching or after using Clearfil Liner Bond 2 self-etching primer (LB2 Primer). Twenty-four non-carious third molars scheduled for extraction from young adult patients (16-30 years old) were used. Conventional Class I cavities (+/- 2 mm deep) were prepared on the occlusal surfaces of all teeth using a cylindrical diamond bur on a high-speed handpiece with copious water spray. To avoid dehydration of the dentin, the smear layer-covered dentin was briefly air-dried for 2 seconds. Cavities were assigned at random to the following groups: Group A: Dentin etched for 15 seconds with 34% phosphoric acid, rinsed for 20 seconds and then briefly air-dried for 2 seconds with oil-free compressed air leaving the surfaces slightly moist. Group B: LB2 Primer was applied to the cavity surfaces for 30 seconds and then briefly air-dried to remove the solvent. Group C: The untreated dentin smear layer was used as a control. In all three groups, the cavities were filled incrementally with a resin-based composite (APX), light curing every increment for 40 seconds. After 30 minutes, the teeth were extracted atraumatically and the samples immediately prepared for evaluation with the transmission electron microscope. The use of a self-etching primer did not produce significant morphological changes in the moist dentin substrate. Adverse morphological conditions where observed when there was an excess water on the dentin surface. Phosphoric acid altered the collagen more severely than the self-etching primer.

Effect of a Cooling Step Treatment on a High-Voltage GaN LED During ICP Dry Etching

NASA Astrophysics Data System (ADS)

Lin, Yen-Sheng; Hsiao, Sheng-Yu; Tseng, Chun-Lung; Shen, Ching-Hsing; Chiang, Jung-Sheng

2017-02-01

In this study, a lower dislocation density for a GaN surface and a reduced current path are observed at the interface of a SiO2 isolation sidewall, using high-resolution transmission electron microscopy. This is grown using a 3-min cooling step treatment during inductivity coupled plasma dry etching. The lower forward voltage is measured, the leakage current decreases from 53nA to 32nA, and the maximum output power increases from 354.8 W to 357.2 W for an input current of 30 mA. The microstructure and the optoelectronic properties of high-voltage light-emitting-diodes is proven to be affected by the cooling step treatment, which allows enough time to release the thermal energy of the SiO2 isolation well.

Observations of Screw Dislocation Driven Growth and Faceting During CVD Homoepitaxy on 4H-SiC On-Axis Mesa Arrays

NASA Technical Reports Server (NTRS)

Neudeck, Philip G.; Trunek, Andrew J.; Powell, J. Anthony; Picard, Yoosuf N.; Twigg, Mark E.

2009-01-01

Previous studies of (0001) homoepitaxial growth carried out on arrays of small-area mesas etched into on-axis silicon-face 4H-SiC wafers have demonstrated that spiral growth emanating from at least one screw dislocation threading the mesa is necessary in order for a mesa to grow taller in the <0001> (c-axis vertical) direction while maintaining 4H stacking sequence [1]. However, even amongst mesas containing the screw dislocation step source necessary for vertical c-axis growth, we have observed striking differences in the height and faceting that evolve during prolonged homoepitaxial growths. This paper summarizes Atomic Force Microscopy (AFM), Electron Channeling Contrast Imaging (ECCI), Scanning Electron Microscopy (SEM), and optical microscopy observations of this phenomenon. These observations support our initially proposed model [2] that the observed large variation (for mesas where 3C-SiC nucleation has not occurred) is related to the lateral positioning of a screw dislocation step source within each etched mesa. When the screw dislocation step source is located close enough to the developing edge/sidewall facet of a mesa, the c-axis growth rate and facet angle are affected by the resulting interaction. In particular, the intersection (or near intersection) of the inward-sloping mesa sidewall facet with the screw dislocation appears to impede the rate at which the spiral provides new steps required for c-axis growth. Also, the inward slope of the sidewall facet during growth (relative to other sidewalls of the same mesa not near the screw dislocation) seems to be impeded by the screw dislocation. In contrast, mesas whose screw dislocations are centrally located grow vertically, but inward sloping sidewall facets shrink the area of the top (0001) growth surface almost to the point of vanishing.

Rubbing time and bonding performance of one-step adhesives to primary enamel and dentin

PubMed Central

Botelho, Maria Paula Jacobucci; Isolan, Cristina Pereira; Schwantz, Júlia Kaster; Lopes, Murilo Baena; de Moraes, Rafael Ratto

2017-01-01

Abstract Objectives: This study investigated whether increasing the concentration of acidic monomers in one-step adhesives would allow reducing their application time without interfering with the bonding ability to primary enamel and dentin. Material and methods: Experimental one-step self-etch adhesives were formulated with 5 wt% (AD5), 20 wt% (AD20), or 35 wt% (AD35) acidic monomer. The adhesives were applied using rubbing motion for 5, 10, or 20 s. Bond strengths to primary enamel and dentin were tested under shear stress. A commercial etch-and-rinse adhesive (Single Bond 2; 3M ESPE) served as reference. Scanning electron microscopy was used to observe the morphology of bonded interfaces. Data were analysed at p<0.05. Results: In enamel, AD35 had higher bond strength when rubbed for at least 10 s, while application for 5 s generated lower bond strength. In dentin, increased acidic monomer improved bonding only for 20 s rubbing time. The etch-and-rinse adhesive yielded higher bond strength to enamel and similar bonding to dentin as compared with the self-etch adhesives. The adhesive layer was thicker and more irregular for the etch-and-rinse material, with no appreciable differences among the self-etch systems. Conclusion: Overall, increasing the acidic monomer concentration only led to an increase in bond strength to enamel when the rubbing time was at least 10 s. In dentin, despite the increase in bond strength with longer rubbing times, the results favoured the experimental adhesives compared to the conventional adhesive. Reduced rubbing time of self-etch adhesives should be avoided in the clinical setup. PMID:29069150

Effect of application mode on interfacial morphology and chemistry between dentin and self-etch adhesives

PubMed Central

Zhang, Ying; Wang, Yong

2012-01-01

Objective To investigate the influence of application mode on the interfacial morphology and chemistry between dentin and self-etch adhesives with different aggressiveness. Methods The occlusal one-third of the crown was removed from un-erupted human third molars, followed by abrading with 600 grit SiC under water. Rectangular dentin slabs were prepared by sectioning the tooth specimens perpendicular to the abraded surfaces. The obtained dentin slabs were treated with one of the two one-step self-etch adhesives: Adper Easy Bond (AEB, PH~2.5) and Adper Prompt L-Pop (APLP, PH~0.8) with (15s, active application) or without (15s, inactive application) agitation. The dentin slabs were fractured and the exposed adhesive/dentin (A/D) interfaces were examined with micro-Raman spectroscopy and scanning electron microscopy (SEM). Results The interfacial morphology, degree of dentin demineralization (DD) and degree of conversion (DC) of the strong self-etch adhesive APLP showed more significant dependence on the application mode than the mild AEB. APLP exhibited inferior bonding at the A/D interface if applied without agitation, evidenced by debonding from the dentin substrate. The DDs and DCs of the APLP with agitation were higher than those of without agitation in the interface, in contrast to the comparable DD and DC values of two AEB specimen groups with different application modes. Raman spectral analysis revealed the important role of chemical interaction between acid monomers of self-etch adhesives and dentin in the above observations. Conclusion The chemical interaction with dentin is especially important for improving the DC of the strong self-etching adhesive at the A/D interface. Agitation could benefit polymerization efficacy of the strong self-etch adhesive through enhancing the chemical interaction with tooth substrate. PMID:23153573

Chlorhexidine diminishes the loss of bond strength over time under simulated pulpal pressure and thermo-mechanical stressing.

PubMed

Campos, Edson Alves; Correr, Gisele Maria; Leonardi, Denise Piotto; Barato-Filho, Flares; Gonzaga, Carla Castiglia; Zielak, João César

2009-02-01

The purpose of this study was to investigate the effects of chlorhexidine (CHX) digluconate at 0.2% and 2% on dentin bonding durability of etch-and-rinse and self-etch adhesive systems. In this study were used 24 extracted non-carious human third-molars. The occlusal surfaces of the molar crowns were removed with a low-speed diamond saw to expose flat dentin surfaces. The tested materials were Single-Bond (SB) (two-step etch-and-rinse adhesive) and Clearfil Tri S Bond (CTSB) (all-in-one self-etch adhesive) used in association or not with CHX at 0.2% and 2%. The bonding systems were applied according to manufacturer's instructions and followed by composite application (Z250). For each condition, half of the specimens was immediately submitted to microtensile test and half of them was submitted to long-term storage of 6 months under simulated pulpal pressure and thermo-mechanical stressing before testing. The data were analyzed using Two-Way ANOVA and Tukey post hoc test (alpha=0.05). Failure patterns of the specimens were observed using scanning electron microscopy. The falling % in bond strength over the 6-month period was: SB control-43.64%; SB/0.2%CHX-23.79%; SB/2%CHX-26.42%; CTSB control-40.94%; CTSB/0.2%CHX-37.07%; CTSB/2%CHX-22.14%. The fracture modes were predominantly adhesive, mainly in the specimens of terminal groups. CXH digluconate at 2% was able to diminish loss of microtensile bond strength over time associated to both etch-and-rinse and self-etch adhesives. Lower concentration of CHX (0.2%) was not able to diminish the loss of bond strength over time when associated to the self-etch adhesive CTSB.

Dentin bond strength and nanoleakage of the adhesive interface after intracoronal bleaching.

PubMed

Cavalli, Vanessa; Sebold, Maicon; Shinohara, Mirela Sanae; Pereira, Patrícia Nóbrega Rodrigues; Giannini, Marcelo

2018-04-01

This study evaluated dentin bond strength (BS) and nanoleakage of non- and pre-etched dentin immediately (T 0 ,), 7 days (T 7 ), and 14 days (T 14 ) after bleaching. Bovine incisors (150) were selected and half of them submitted to intrapulpal dentin etching (e). Non- and pre-etched dentin were subjected to the following (n = 15): no bleaching/control (C); 35% carbamide peroxide (CP); 35% hydrogen peroxide (35% HP); 25% hydrogen peroxide (25% HP); and sodium perborate (SP). Bleaching agents were applied to the pulp chamber four times within a 72-h interval. Afterwards, pulp chamber dentin was prepared for the BS test at different evaluation times (n = 5): T 0 , T 7 , and T 14 . Composite blocks were built on pulp chamber and sectioned in slices. Slices were reduced to an hour-glass shape with a cross-sectional area of 0.8 mm 2 and submitted to microtensile BS test. Two additional specimens for each group were prepared for nanoleakage evaluation by transmission electron microscopy (TEM). Results were analyzed by ANOVA (two-way) and Dunnett's test (p < .05). BS decreased immediately after intracoronal bleaching for both sound and pre-etched dentin (p < .05). At T 14 , the BS of non-etched bleached dentin increased for all groups, whereas the pre-etched SPe group presented BS similar to the Ce. Nanoleakage within the hybrid layer was perceptible immediately after bleaching, although a decrease in nanoleakage was observed for all groups at T 14 . Adhesive restorations should be performed 7-14 days after bleaching, according to the bleaching agent used. Intracoronal bleaching should be performed preferably with sodium perborate if previous dentin etching is applied. © 2018 Wiley Periodicals, Inc.

Surface-pattern geometry, topography, and chemical modifications during KrF excimer laser micro-drilling of p-type Si (111) wafers in ambient environment of HCl fumes in air

NASA Astrophysics Data System (ADS)

Zakria Butt, Muhammad; Saher, Sobia; Waqas Khaliq, Muhammad; Siraj, Khurram

2016-11-01

Eight mirror-like polished p-type Si (111) wafers were irradiated with 100, 200, 300, 400, 800, 1200, 1600, and 2000 KrF excimer laser pulses in ambient environment of HCl fumes in air. The laser parameters were: wavelength = 248 nm, pulse width = 20 ns, pulse energy = 20 mJ, and repetition rate = 20 Hz. For each set of laser pulses, characterization of the rectangular etched patterns formed on target surface was done by optical/scanning electron microscopy, XRD, and EDX techniques. The average etched depth increased with the increase in number of laser pulses from 100 to 2000 in accord with Sigmoidal (Boltzmann) function, whereas the average etch rate followed an exponential decay with the increase in number of laser pulses. However, the etched area, maximum etched depth, and maximum etch rate were found to increase linearly with the number of laser pulses, but the rate of increase was faster for 100-400 laser pulses (region I) than that for 800-2000 laser pulses (region II). The elemental composition for each etched-pattern determined by EDX shows that both O and Cl contents increase progressively with the increase in the number of laser shots in region I. However, in region II both O and Cl contents attain saturation values of about 39.33 wt.% and 0.14 wt.%, respectively. Perforation of Si wafers was achieved on irradiation with 1200-2000 laser pulses. XRD analysis confirmed the formation of SiO2, SiCl2 and SiCl4 phases in Si (111) wafers due to chemical reaction of silicon with both HCl fumes and oxygen in air.

Effect of thermal aging on the tensile bond strength at reduced areas of seven current adhesives.

PubMed

Baracco, Bruno; Fuentes, M Victoria; Garrido, Miguel A; González-López, Santiago; Ceballos, Laura

2013-07-01

The purpose of this study was to determine the micro-tensile bond strength (MTBS) to dentin of seven adhesive systems (total and self-etch adhesives) after 24 h and 5,000 thermocycles. Dentin surfaces of human third molars were exposed and bonded with two total-etch adhesives (Adper Scotchbond 1 XT and XP Bond), two two-step self-etch adhesives (Adper Scotchbond SE and Filtek Silorane Adhesive System) and three one-step self-etch adhesives (G-Bond, Xeno V and Bond Force). All adhesive systems were applied following manufacturers' instructions. Composite buildups were constructed and the bonded teeth were then stored in water (24 h, 37 °C) or thermocycled (5,000 cycles) before being sectioned and submitted to MTBS test. Two-way ANOVA and subsequent comparison tests were applied at α = 0.05. Characteristic de-bonded specimens were analyzed using scanning electron microscopy (SEM). After 24 h water storage, MTBS values were highest with XP Bond, Adper Scotchbond 1 XT, Filtek Silorane Adhesive System and Adper Scotchbond SE and lowest with the one-step self-etch adhesives Bond Force, Xeno V and G-Bond. After thermocycling, MTBS values were highest with XP Bond, followed by Filtek Silorane Adhesive System, Adper Scotchbond SE and Adper Scotchbond 1 XT and lowest with the one-step self-etch adhesives Bond Force, Xeno V and G-Bond. Thermal aging induced a significant decrease in MTBS values with all adhesives tested. The resistance of resin-dentin bonds to thermal-aging degradation was material dependent. One-step self-etch adhesives obtained the lowest MTBS results after both aging treatments, and their adhesive capacity was significantly reduced after thermocycling.

In situ photoacoustic characterization for porous silicon growing: Detection principles

NASA Astrophysics Data System (ADS)

Ramirez-Gutierrez, C. F.; Castaño-Yepes, J. D.; Rodriguez-García, M. E.

2016-05-01

There are a few methodologies for monitoring the in-situ formation of Porous Silicon (PS). One of the methodologies is photoacoustic. Previous works that reported the use of photoacoustic to study the PS formation do not provide the physical explanation of the origin of the signal. In this paper, a physical explanation of the origin of the photoacoustic signal during the PS etching is provided. The incident modulated radiation and changes in the reflectance are taken as thermal sources. In this paper, a useful methodology is proposed to determine the etching rate, porosity, and refractive index of a PS film by the determination of the sample thickness, using scanning electron microscopy images. This method was developed by carrying out two different experiments using the same anodization conditions. The first experiment consisted of growth of the samples with different etching times to prove the periodicity of the photoacoustic signal, while the second one considered the growth samples using three different wavelengths that are correlated with the period of the photoacoustic signal. The last experiment showed that the period of the photoacoustic signal is proportional to the laser wavelength.

Pyramidal pits created by single highly charged ions in BaF{sub 2} single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

El-Said, A. S.; Physics Department, Faculty of Science, Mansoura University, 35516 Mansoura; Heller, R.

2010-07-15

In various insulators, the impact of individual slow highly charged ions (eV-keV) creates surface nanostructures, whose size depends on the deposited potential energy. Here we report on the damage created on a cleaved BaF{sub 2} (111) surface by irradiation with 4.5xq keV highly charged xenon ions from a room-temperature electron-beam ion trap. Up to charge states q=36, no surface topographic changes on the BaF{sub 2} surface are observed by scanning force microscopy. The hidden stored damage, however, can be made visible using the technique of selective chemical etching. Each individual ion impact develops into a pyramidal etch pits, as canmore » be concluded from a comparison of the areal density of observed etch pits with the applied ion fluence (typically 10{sup 8} ions/cm{sup 2}). The dimensional analysis of the measured pits reveals the significance of the deposited potential energy in the creation of lattice distortions/defects in BaF{sub 2}.« less

Morphological and chemical characteristics of different titanium surfaces treated by bicarbonate and glycine powder air abrasive systems.

PubMed

Menini, Maria; Piccardo, Paolo; Baldi, Domenico; Dellepiane, Elena; Pera, Paolo

2015-02-01

This in vitro study investigated possible morphological and chemical changes induced by glycine or sodium bicarbonate powder air polishing on machined and acid-etched titanium surfaces. The glycine powder (granulometry <65 μm) and sodium bicarbonate powder (granulometry <150 μm) were applied on 2 machined healing abutments and on 2 acid-etched healing abutments. The samples were characterized by scanning electron microscopy coupled with energy dispersive x-ray spectroscopy. The analyses were performed at different steps: (1) as received, right after opening the abutment packaging; (2) after 20 minutes air exposure; (3) after aging in artificial saliva; (4) after glycine or sodium bicarbonate powder air polishing for 5 seconds; (5) after repetition of steps 3 and 4 with longer time of polishing (20 seconds). Air polishing using glycine and sodium bicarbonate powder seemed to be safe for professional oral hygiene of titanium dental implants, although acid-etched abutments and abutments treated with bicarbonate harbored more salts. This might indicate a greater plaque accumulation in a clinical situation. However, this result has to be investigated in vivo to understand its clinical relevance.

Effect of Cl2 plasma treatment and annealing on vanadium based metal contacts to Si-doped Al0.75Ga0.25N

NASA Astrophysics Data System (ADS)

Lapeyrade, Mickael; Alamé, Sabine; Glaab, Johannes; Mogilatenko, Anna; Unger, Ralph-Stephan; Kuhn, Christian; Wernicke, Tim; Vogt, Patrick; Knauer, Arne; Zeimer, Ute; Einfeldt, Sven; Weyers, Markus; Kneissl, Michael

2017-09-01

In order to understand the electrical properties of V/Al/Ni/Au metal contacts to Si-doped Al0.75Ga0.25N layers, X-ray photoelectron spectroscopy analysis was performed on differently treated AlGaN:Si surfaces before metal deposition, and transmission electron microscopy was used to study the semiconductor-metal interface after contact annealing at 900 °C. Cl2 plasma etching of AlGaN increases the aluminum/nitrogen ratio at the surface, and Al oxide or oxynitride is always formed by any surface treatment applied after etching. After contact annealing, a complex interface structure including amorphous AlOx and different metal phases such as Al-Au-Ni, V-Al, and V2N were found. The electrical properties of the contacts were determined by thermionic emission and/or thermionic field emission in the low voltage regime. Nearly ohmic contacts on AlGaN surfaces exposed to a Cl2 plasma were only obtained by annealing the sample at a temperature of 815 °C under N2/NH3 prior to metallization. By this treatment, the oxygen contamination on the surface could be minimized, resulting in a larger semiconductor area to be in direct contact with metal phases such as Al-rich Al-Au-Ni or V-Al and leading to a contact resistivity of 2.5 × 10-2 Ω cm2. This treatment can be used to significantly reduce the operating voltage of current deep ultraviolet light emitting diodes which will increase their wall plug efficiency and lower the thermal stress during their operation.

Low energy electron irradiation induced carbon etching: Triggering carbon film reacting with oxygen from SiO{sub 2} substrate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Cheng; Key Laboratory of Optoelectronic Devices and Systems of Ministry of Education and Guangdong Province, College of Optoelectronic Engineering, Shenzhen University, Shenzhen 518060; Wang, Chao, E-mail: cwang367@szu.edu.cn, E-mail: dfdiao@szu.edu.cn

2016-08-01

We report low-energy (50–200 eV) electron irradiation induced etching of thin carbon films on a SiO{sub 2} substrate. The etching mechanism was interpreted that electron irradiation stimulated the dissociation of the carbon film and SiO{sub 2}, and then triggered the carbon film reacting with oxygen from the SiO{sub 2} substrate. A requirement for triggering the etching of the carbon film is that the incident electron penetrates through the whole carbon film, which is related to both irradiation energy and film thickness. This study provides a convenient electron-assisted etching with the precursor substrate, which sheds light on an efficient pathway to themore » fabrication of nanodevices and nanosurfaces.« less

Surface Modification of Ti-35Nb-10Ta-1.5Fe by the Double Acid-Etching Process

PubMed Central

Amigó, Angélica

2018-01-01

Surface topography and composition influence the osteoblastic proliferation and osseointegration rates, which favor the biomechanical stability of bone anchoring and implants. In recent years, beta titanium alloys have been developed, and are composed of biocompatible elements, have low elastic modulus, high corrosion resistance, and mechanical properties to improve the long performance behavior of biomaterials. In the present research, the influence of the acid-etching process was studied in Ti6Al4V ELI and Ti35Nb10Ta1.5Fe. Samples were etched in a two-step acid treatment. Surface roughness parameters were quantified under a confocal microscope, topography was studied by scanning electron microscopy, and surface composition was analyzed with energy dispersive X-ray spectroscopy. The results revealed that the two-step acid treatment changes the topography of the β alloy, increases the surface area, and changes the chemical composition of the surface. Two differentiated regions were identified in the Ti35Nb10Ta1.5Fe alloy after the acid-etching process: The α + β region with higher values of mean roughness due to the lower chemical resistance of this region; and the β region with lower values of roughness parameters. PMID:29587427

Effect of Minocycline on the Durability of Dentin Bonding Produced with Etch-and-Rinse Adhesives.

PubMed

Loguercio, A D; Stanislawczuk, R; Malaquias, P; Gutierrez, M F; Bauer, J; Reis, A

2016-01-01

To evaluate the effect of minocycline and chlorhexidine pretreatment of acid-etched dentin on the longevity of resin-dentin bond strength (μTBS) and nanoleakage of two-step etch-and-rinse adhesives. Before application of Prime & Bond NT and Adper Single Bond 2 in occlusal dentin, the dentin surfaces were treated with 37% phosphoric acid, rinsed, air-dried, and rewetted with water (control group), 2% minocycline, or 2% chlorexidine digluconate. Composite buildups were constructed incrementally, and specimens were longitudinally sectioned to obtain bonded sticks (0.8 mm 2 ) to be tested in tension (0.5 mm/min) immediately or after 24 months of water storage. For nanoleakage, two specimens of each tooth/period were immersed in the silver nitrate solution, photo-developed, and polished with SiC paper for analysis under energy-dispersive X-ray spectroscopy/scanning electron microscopy. Reductions of the μTBS and increases in the nanoleakage were observed for both adhesives when the rewetting procedure was performed with water. Stable bonds were observed for the 2% minocycline and 2% chlorexidine digluconate groups after 24 months. The use of 2% minocycline as pretreatment of acid-etched dentin is one alternative to retard the degradation of resin-dentin interfaces over a 24-month period as well as 2% chlorexidine digluconate.

Molecular beam epitaxy growth of high electron mobility InAs/AlSb deep quantum well structure

NASA Astrophysics Data System (ADS)

Wang, Juan; Wang, Guo-Wei; Xu, Ying-Qiang; Xing, Jun-Liang; Xiang, Wei; Tang, Bao; Zhu, Yan; Ren, Zheng-Wei; He, Zhen-Hong; Niu, Zhi-Chuan

2013-07-01

InAs/AlSb deep quantum well (QW) structures with high electron mobility were grown by molecular beam epitaxy (MBE) on semi-insulating GaAs substrates. AlSb and Al0.75Ga0.25Sb buffer layers were grown to accommodate the lattice mismatch (7%) between the InAs/AlSb QW active region and GaAs substrate. Transmission electron microscopy shows abrupt interface and atomic force microscopy measurements display smooth surface morphology. Growth conditions of AlSb and Al0.75Ga0.25Sb buffer were optimized. Al0.75Ga0.25Sb is better than AlSb as a buffer layer as indicated. The sample with optimal Al0.75Ga0.25Sb buffer layer shows a smooth surface morphology with root-mean-square roughness of 6.67 Å. The electron mobility has reached as high as 27 000 cm2/Vs with a sheet density of 4.54 × 1011/cm2 at room temperature.

Influence of laboratory degradation methods and bonding application parameters on microTBS of self-etch adhesives to dentin.

PubMed

Erhardt, Maria Carolina G; Pisani-Proença, Jatyr; Osorio, Estrella; Aguilera, Fátima S; Toledano, Manuel; Osorio, Raquel

2011-04-01

To evaluate the laboratory resistance to degradation and the use of different bonding treatments on resin-dentin bonds formed with three self-etching adhesive systems. Flat, mid-coronal dentin surfaces from extracted human molars were bonded according to manufacturer's directions and submitted to two challenging regimens: (A) chemical degradation with 10% NaOC1 immersion for 5 hours; and (B) fatigue loading at 90 N using 50,000 cycles at 3.0 Hz. Additional dentin surfaces were bonded following four different bonding application protocols: (1) according to manufacturer's directions; (2) acid-etched with 36% phosphoric acid (H3PO4) for 15 seconds; (3) 10% sodium hypochlorite (NaOClaq) treated for 2 minutes, after H3PO4-etching; and (4) doubling the application time of the adhesives. Two one-step self-etch adhesives (an acetone-based: Futurabond/FUT and an ethanol-based: Futurabond NR/FNR) and a two-step self-etch primer system (Clearfil SE Bond/CSE) were examined. Specimens were sectioned into beams and tested for microtensile bond strength (microTBS). Selected debonded specimens were observed under scanning electron microscopy (SEM). Data (MPa) were analyzed by ANOVA and multiple comparisons tests (alpha= 0.05). microTBS significantly decreased after chemical and mechanical challenges (P< 0.05). CSE showed higher microTBS than the other adhesive systems, regardless the bonding protocol. FUT attained the highest microTBS after doubling the application time. H3PO4 and H3PO4 + NaOCl pretreatments significantly decreased bonding efficacy of the adhesives.

Effects of processing history on the evolution of surface damage layer and dislocation substructure in large grain niobium cavities

DOE PAGES

Kang, D.; Bieler, T. R.; Compton, C.

2015-12-16

Large grain niobium (Nb) is being investigated for fabricating superconducting radiofrequency cavities as an alternative to the traditional approach using fine grain polycrystalline Nb sheets. Past studies have identified a surface damage layer on fine grain cavities due to deep drawing and demonstrated the necessity for chemical etching on the surface. However, the origin of and depth of the damage layer are not well understood, and similar exploration on large grain cavities is lacking. In this work, electron backscatter diffraction (EBSD) was used to examine the cross sections at the equator and iris of a half cell deep drawn frommore » a large grain Nb ingot slice. The results indicate that the damage (identified by a high density of geometrically necessary dislocations) depends on crystal orientations, is different at the equator and iris, and is present through the full thickness of a half cell in some places. After electron backscatter diffraction, the specimens were heat treated at 800 °C or 1000 °C for two hours, and the same areas were reexamined. A more dramatic decrease in dislocation content was observed at the iris than the equator, where some regions exhibited no change. The specimens were then etched and examined again, to determine if the subsurface region behaved differently than the surface. As a result, little change in the dislocation substructure was observed, suggesting that the large grain microstructure is retained with a normal furnace anneal.« less

Fabrication of high aspect ratio tungsten nanostructures on ultrathin c-Si membranes for extreme UV applications

NASA Astrophysics Data System (ADS)

Delachat, F.; Le Drogoff, B.; Constancias, C.; Delprat, S.; Gautier, E.; Chaker, M.; Margot, J.

2016-01-01

In this work, we demonstrate a full process for fabricating high aspect ratio diffraction optics for extreme ultraviolet lithography. The transmissive optics consists in nanometer scale tungsten patterns standing on flat, ultrathin (100 nm) and highly transparent (>85% at 13.5 nm) silicon membranes (diameter of 1 mm). These tungsten patterns were achieved using an innovative pseudo-Bosch etching process based on an inductively coupled plasma ignited in a mixture of SF6 and C4F8. Circular ultra-thin Si membranes were fabricated through a state-of-the-art method using direct-bonding with thermal difference. The silicon membranes were sputter-coated with a few hundred nanometers (100-300 nm) of stress-controlled tungsten and a very thin layer of chromium. Nanoscale features were written in a thin resist layer by electron beam lithography and transferred onto tungsten by plasma etching of both the chromium hard mask and the tungsten layer. This etching process results in highly anisotropic tungsten features at room temperature. The homogeneity and the aspect ratio of the advanced pattern transfer on the membranes were characterized with scanning electron microscopy after focus ion beam milling. An aspect ratio of about 6 for 35 nm size pattern is successfully obtained on a 1 mm diameter 100 nm thick Si membrane. The whole fabrication process is fully compatible with standard industrial semiconductor technology.

Efficient etching-free transfer of high quality, large-area CVD grown graphene onto polyvinyl alcohol films

NASA Astrophysics Data System (ADS)

Marta, Bogdan; Leordean, Cosmin; Istvan, Todor; Botiz, Ioan; Astilean, Simion

2016-02-01

Graphene transfer is a procedure of paramount importance for the production of graphene-based electronic devices. The transfer procedure can affect the electronic properties of the transferred graphene and can be detrimental for possible applications both due to procedure induced defects which can appear and due to scalability of the method. Hence, it is important to investigate new transfer methods for graphene that are less time consuming and show great promise. In the present study we propose an efficient, etching-free transfer method that consists in applying a thin polyvinyl alcohol layer on top of the CVD grown graphene on Cu and then peeling-off the graphene onto the polyvinyl alcohol film. We investigate the quality of the transferred graphene before and after the transfer, using Raman spectroscopy and imaging as well as optical and atomic force microscopy techniques. This simple transfer method is scalable and can lead to complete transfer of graphene onto flexible and transparent polymer support films without affecting the quality of the graphene during the transfer procedure.

Nanoclay/Polymer Composite Powders for Use in Laser Sintering Applications: Effects of Nanoclay Plasma Treatment

NASA Astrophysics Data System (ADS)

Almansoori, Alaa; Majewski, Candice; Rodenburg, Cornelia

2017-11-01

Plasma-etched nanoclay-reinforced Polyamide 12 (PA12) powder is prepared with its intended use in selective laser sintering (LS) applications. To replicate the LS process we present a downward heat sintering (DHS) process, carried out in a hot press, to fabricate tensile test specimens from the composite powders. The DHS parameters are optimized through hot stage microscopy, which reveal that the etched clay (EC)-based PA12 (EC/PA12) nanocomposite powder melts at a temperature 2°C higher than that of neat PA12, and 1-3°C lower than that of the nonetched clay-based nanocompsite (NEC/PA12 composite). We show that these temperature differences are critical to successful LS. The distribution of EC and NEC onto PA12 is investigated by scanning electron microscopy (SEM). SEM images show clearly that the plasma treatment prevents the micron-scale aggregation of the nanoclay, resulting in an improved elastic modulus of EC/PA12 when compared with neat PA12 and NEC/PA12. Moreover, the reduction in elongation at break for EC/PA12 is less pronounced than for NEC/PA12.

Uniformly thinned optical fibers produced via HF etching with spectral and microscopic verification.

PubMed

Bal, Harpreet K; Brodzeli, Zourab; Dragomir, Nicoleta M; Collins, Stephen F; Sidiroglou, Fotios

2012-05-01

A method for producing uniformly thinned (etched) optical fibers is described, which can also be employed to etch optical fibers containing a Bragg grating (FBG) uniformly for evanescent-field-based sensing and other applications. Through a simple modification of this method, the fabrication of phase-shifted FBGs based on uneven etching is also shown. The critical role of how a fiber is secured is shown, and the success of the method is illustrated, by differential interference contrast microscopy images of uniformly etched FBGs. An etched FBG sensor for the monitoring of the refractive index of different glycerin solutions is demonstrated.

Deep inductively coupled plasma etching of ELO-GaN grown with high fill factor

NASA Astrophysics Data System (ADS)

Gao, Haiyong; Lee, Jaesoong; Ni, Xianfeng; Leach, Jacob; Özgür, Ümit; Morkoç, Hadis

2011-02-01

The epitaxial lateral overgrowth (ELO) gallium nitride (GaN) was grown with high fill factor using metal organic chemical vapor deposition (MOCVD). The inductively coupled plasma (ICP) etching of ELO-GaN based on Cl2/Ar/SiCl4 gas mixture was performed. Surface properties of ELO-GaN subjected to ICP etching have been investigated and optimized etching condition in ELO-GaN with ICP etching is presented. Radiofrequency (RF) power and the flow rate of Cl2 gas were modified during the experiments. The window region, wing region and the edge region of ELO-GaN pattern present different etching characteristics. Different etching conditions were studied to get the minimized plasma-induced damage, relatively high etching rates, and excellent surface profiles. Etch depths of the etched ELO-GaN with smooth surface up to about 19 μm were achieved. The most suitable three-step etching condition is discussed with the assessment based on the morphology observation of the etched surface of ELO-GaN patterns.

Ultrastructure in frozen/etched saline solutions: on the internal cleansing of ice.

PubMed

Menger, Fredric M; Galloway, Ashley L; Chlebowski, Mary E; Apkarian, Robert P

2004-05-19

Seawater, with its 3.5% salt content, freezes into hexagonal ice (Ih) that encloses concentrated brine within its matrix. When unsubmerged sea ice reaches a certain height and temperature, the brine drains downward through narrow channels. This mechanism was now modeled by frozen 2-3.5% saline as investigated by cryo-etch high-resolution secondary electron microscopy. Thus, saline was either plunge-frozen in liquid ethane at -183 degrees C or else high-pressure frozen to -105 degrees C in 5-6 ms. Ice from a freshly exposed surface was then subjected to a high-vacuum sublimation ("etching"), a procedure that removes pure bulk ice in preference to ice from frozen hydrated salt. After chromium-coating the etched surface with a 2-nm film, the sample was examined by cryo-HRSEM. Granular icy "fences" were seen surrounding empty areas where amorphous ice had originally resided. Since the fences, about 1-2 mum high, survived the etching, it is likely that they consist of frozen brine. The presence of such fences suggests that, during freezing, saline can purge itself of salt with remarkable speed (5-6 ms). Alternatively, channels (perhaps routed around submicroscopic crystallites of cubic ice (Ic) embedded in the amorphous ice at -105 degrees C) can guide the migration of salt to the periphery of ice patches. Macromolecules fail to form fences because they diffuse too slowly or because they are too large to pass through the channels.

Formation of silicon nanowire packed films from metallurgical-grade silicon powder using a two-step metal-assisted chemical etching method.

PubMed

Ouertani, Rachid; Hamdi, Abderrahmen; Amri, Chohdi; Khalifa, Marouan; Ezzaouia, Hatem

2014-01-01

In this work, we use a two-step metal-assisted chemical etching method to produce films of silicon nanowires shaped in micrograins from metallurgical-grade polycrystalline silicon powder. The first step is an electroless plating process where the powder was dipped for few minutes in an aqueous solution of silver nitrite and hydrofluoric acid to permit Ag plating of the Si micrograins. During the second step, corresponding to silicon dissolution, we add a small quantity of hydrogen peroxide to the plating solution and we leave the samples to be etched for three various duration (30, 60, and 90 min). We try elucidating the mechanisms leading to the formation of silver clusters and silicon nanowires obtained at the end of the silver plating step and the silver-assisted silicon dissolution step, respectively. Scanning electron microscopy (SEM) micrographs revealed that the processed Si micrograins were covered with densely packed films of self-organized silicon nanowires. Some of these nanowires stand vertically, and some others tilt to the silicon micrograin facets. The thickness of the nanowire films increases from 0.2 to 10 μm with increasing etching time. Based on SEM characterizations, laser scattering estimations, X-ray diffraction (XRD) patterns, and Raman spectroscopy, we present a correlative study dealing with the effect of the silver-assisted etching process on the morphological and structural properties of the processed silicon nanowire films.

Formation of silicon nanowire packed films from metallurgical-grade silicon powder using a two-step metal-assisted chemical etching method

PubMed Central

2014-01-01

In this work, we use a two-step metal-assisted chemical etching method to produce films of silicon nanowires shaped in micrograins from metallurgical-grade polycrystalline silicon powder. The first step is an electroless plating process where the powder was dipped for few minutes in an aqueous solution of silver nitrite and hydrofluoric acid to permit Ag plating of the Si micrograins. During the second step, corresponding to silicon dissolution, we add a small quantity of hydrogen peroxide to the plating solution and we leave the samples to be etched for three various duration (30, 60, and 90 min). We try elucidating the mechanisms leading to the formation of silver clusters and silicon nanowires obtained at the end of the silver plating step and the silver-assisted silicon dissolution step, respectively. Scanning electron microscopy (SEM) micrographs revealed that the processed Si micrograins were covered with densely packed films of self-organized silicon nanowires. Some of these nanowires stand vertically, and some others tilt to the silicon micrograin facets. The thickness of the nanowire films increases from 0.2 to 10 μm with increasing etching time. Based on SEM characterizations, laser scattering estimations, X-ray diffraction (XRD) patterns, and Raman spectroscopy, we present a correlative study dealing with the effect of the silver-assisted etching process on the morphological and structural properties of the processed silicon nanowire films. PMID:25349554

Shear Bond Strength of Superficial, Intermediate and Deep Dentin In Vitro with Recent Generation Self-etching Primers and Single Nano Composite Resin.

PubMed

Singh, Kulshrest; Naik, Rajaram; Hegde, Srinidhi; Damda, Aftab

2015-01-01

This in vitro study is intended to compare the shear bond strength of recent self-etching primers to superficial, intermediate, and deep dentin levels. All teeth were sectioned at various levels and grouped randomly into two experimental groups and two control groups having three subgroups. The experimental groups consisted of two different dentin bonding system. The positive control group consisted of All Bond 2 and the negative control group was without the bonding agent. Finally, the specimens were subjected to shear bond strength study under Instron machine. The maximum shear bond strengths were noted at the time of fracture. The results were statistically analyzed. Comparing the shear bond strength values, All Bond 2 (Group III) demonstrated fairly higher bond strength values at different levels of dentin. Generally comparing All Bond 2 with the other two experimental groups revealed highly significant statistical results. In the present investigation with the fourth generation, higher mean shear bond strength values were recorded compared with the self-etching primers. When intermediate dentin shear bond strength was compared with deep dentin shear bond strength statistically significant results were found with Clearfil Liner Bond 2V, All Bond 2 and the negative control. There was a statistically significant difference in shear bond strength values both with self-etching primers and control groups (fourth generation bonding system and without bonding system) at superficial, intermediate, and deep dentin. There was a significant fall in bond strength values as one reaches deeper levels of dentin from superficial to intermediate to deep.

Characterization of the NEXT Hollow Cathode Inserts After Long-Duration Testing

NASA Technical Reports Server (NTRS)

Mackey, J.; Shastry, R.; Soulas, G.

2017-01-01

Hollow dispenser cathode inserts are a critical element of electric propulsion systems, and should therefore be well understood during long term operation to ensure reliable system performance. This work destructively investigated cathode inserts from the NEXT long-duration test which demonstrated 51,184 hours of high-voltage operation, 918 kg of propellant throughput, and 35.5 MN-s of total impulse. The characterization methods used include scanning electron microscopy with energy dispersive spectroscopy and X-ray diffraction. Microscopy analysis has been performed on fractured surfaces, emission surfaces, and metallographically polished cross-sections of post-test inserts and unused inserts. Impregnate distribution, etch region thickness, impregnate chemical content, emission surface topography, and emission surface phase identification are the primary factors investigated.

Lateral overgrowth of diamond film on stripes patterned Ir/HPHT-diamond substrate

NASA Astrophysics Data System (ADS)

Wang, Yan-Feng; Chang, Xiaohui; Liu, Zhangcheng; Liu, Zongchen; Fu, Jiao; Zhao, Dan; Shao, Guoqing; Wang, Juan; Zhang, Shaopeng; Liang, Yan; Zhu, Tianfei; Wang, Wei; Wang, Hong-Xing

2018-05-01

Epitaxial lateral overgrowth (ELO) of diamond films on patterned Ir/(0 0 1)HPHT-diamond substrates have been carried out by microwave plasma CVD system. Ir/(0 0 1)HPHT-diamond substrates are fabricated by photolithographic and magnetron sputtering technique. The morphology of the as grown ELO diamond film is characterized by optical microscopy and scanning electronic microscopy. The quality and stress of the ELO diamond film are investigated by surface etching pit density and micro-Raman spectroscopy. Two ultraviolet photodetectors are fabricated on ELO diamond area and non-ELO diamond area prepared on same substrate, and that one on ELO diamond area indicates better photoelectric properties. All results indicate quality of ELO diamond film is improved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Railsback, Justin; Pearce, Ryan; Sarac, Mehmet

Vertically aligned carbon nanofibers (VACNFs) are synthesized on 3003 aluminum substrates by direct current plasma enhanced chemical vapor deposition. Chemically synthesized nickel nanoparticles were used as the catalyst for growth. The silicon containing coating (SiNx) typically produced when VACNFs are grown on silicon was produced by adding silicon microparticles prior to growth. The fiber array was transferred to PDMS by spin casting a layer on the grown substrates, curing the PDMS, and etching away the aluminum in KOH. Energy dispersive x-ray spectroscopy, scanning electron microscopy, and fluorescence microscopy data are provided. The free standing array in PDMS was then loadedmore » with pVENUS-C1 plasmid and human brain microcapillary endothelial cells (HCMECHBMEC)/d3 cells were successfully impalefected with the plasmid.« less

Characteristics of InN epilayers grown with H2-assistance

NASA Astrophysics Data System (ADS)

Zhou, Jin; Li, Jinchai; Lu, Shiqiang; Kang, Junyong; Lin, Wei

2017-11-01

A series of InN films were grown on GaN-on-sapphire template with H2 pulse flow by metal organic vapor phase epitaxy. The scanning electron microscopy and atomic force microscopy observations demonstrate that the smooth surface has been achieved. The X-ray diffraction and Raman spectra measurements indicate that InN layers experience stronger accommodated compressive stress, resulting in a larger fraction of (002) oriented InN grains. On the basics of the first-principles calculations, these features can be understand as competition between N-penetrating effect with the assistance of the H atom and the etching effect of H2. Finally, the absorption spectra in conjunction with simulated results reveal that the band gap energy predominantly increase with increasing compressive strain.

Spherical nitrogen-doped hollow mesoporous carbon as an efficient bifunctional electrocatalyst for Zn-air batteries

NASA Astrophysics Data System (ADS)

Hadidi, Lida; Davari, Elaheh; Iqbal, Muhammad; Purkait, Tapas K.; Ivey, Douglas G.; Veinot, Jonathan G. C.

2015-12-01

Materials based upon porous carbon have gained considerable attention due to their high surface area, electric conductivity, thermal and chemical stability, low density, and availability. These superior properties make them ideal for diverse applications. Doping these carbon nanostructures holds promise of designing the properties of these structures and opening the door to practical applications. Herein, we report the preparation of hollow N-doped mesoporous carbon (HMC) spheres fabricated via polymerization and carbonization of dopamine on a sacrificial spherical SiO2 template that is removed upon hydrofluoric acid etching. The morphology and structural features of these HMCs were evaluated using scanning electron microscopy and transmission electron microscopy and the N-doping (7.1 at%) was confirmed by X-ray photoelectron spectroscopy (XPS). The oxygen reduction/evolution reaction (ORR/OER) performance of N-doped HMC was evaluated using rotating disk electrode (RDE) voltammetry in an alkaline electrolyte. N-doped HMC demonstrated a high ORR onset potential of -0.055 V (vs. Hg/HgO) and excellent stability. The outstanding bifunctional activity was implemented in a practical Zn-air battery (ZAB), which exhibited a small charge-discharge voltage polarization of 0.89 V and high stability over repeated cycling.Materials based upon porous carbon have gained considerable attention due to their high surface area, electric conductivity, thermal and chemical stability, low density, and availability. These superior properties make them ideal for diverse applications. Doping these carbon nanostructures holds promise of designing the properties of these structures and opening the door to practical applications. Herein, we report the preparation of hollow N-doped mesoporous carbon (HMC) spheres fabricated via polymerization and carbonization of dopamine on a sacrificial spherical SiO2 template that is removed upon hydrofluoric acid etching. The morphology and structural features of these HMCs were evaluated using scanning electron microscopy and transmission electron microscopy and the N-doping (7.1 at%) was confirmed by X-ray photoelectron spectroscopy (XPS). The oxygen reduction/evolution reaction (ORR/OER) performance of N-doped HMC was evaluated using rotating disk electrode (RDE) voltammetry in an alkaline electrolyte. N-doped HMC demonstrated a high ORR onset potential of -0.055 V (vs. Hg/HgO) and excellent stability. The outstanding bifunctional activity was implemented in a practical Zn-air battery (ZAB), which exhibited a small charge-discharge voltage polarization of 0.89 V and high stability over repeated cycling. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06028a

Ultradeep electron cyclotron resonance plasma etching of GaN

DOE PAGES

Harrison, Sara E.; Voss, Lars F.; Torres, Andrea M.; ...

2017-07-25

Here, ultradeep (≥5 μm) electron cyclotron resonance plasma etching of GaN micropillars was investigated. Parametric studies on the influence of the applied radio-frequency power, chlorine content in a Cl 2/Ar etch plasma, and operating pressure on the etch depth, GaN-to-SiO 2 selectivity, and surface morphology were performed. Etch depths of >10 μm were achieved over a wide range of parameters. Etch rates and sidewall roughness were found to be most sensitive to variations in RF power and % Cl 2 in the etch plasma. Selectivities of >20:1 GaN:SiO 2 were achieved under several chemically driven etch conditions where a maximummore » selectivity of ~39:1 was obtained using a 100% Cl 2 plasma. The etch profile and (0001) surface morphology were significantly influenced by operating pressure and the chlorine content in the plasma. Optimized etch conditions yielded >10 μm tall micropillars with nanometer-scale sidewall roughness, high GaN:SiO 2 selectivity, and nearly vertical etch profiles. These results provide a promising route for the fabrication of ultradeep GaN microstructures for use in electronic and optoelectronic device applications. In addition, dry etch induced preferential crystallographic etching in GaN microstructures is also demonstrated, which may be of great interest for applications requiring access to non- or semipolar GaN surfaces.« less

In vitro longevity of bonding properties of universal adhesives to dentin.

PubMed

Muñoz, M A; Luque-Martinez, I; Malaquias, P; Hass, V; Reis, A; Campanha, N H; Loguercio, A D

2015-01-01

To evaluate the immediate and 6-month resin-dentin bond strength (μTBS) and nanoleakage (NL) of universal adhesives that contain or do not contain methacryloyloxydecyl dihydrogen phosphate (MDP) and are used in the etch-and-rinse and self-etch strategies. Forty caries-free extracted third molars were divided into eight groups for μTBS (n=5). The groups were bonded with the Clearfil SE Bond (CSE) and Adper Single Bond 2 (SB) as controls; Peak Universal, self-etch (PkSe) and etch-and rinse (PkEr); Scotchbond Universal Adhesive, self-etch (ScSe) and etch-and-rinse (ScEr); and All Bond Universal, self-etch (AlSe) and etch-and-rinse (AlEr). After composite restorations, specimens were longitudinally sectioned to obtain resin-dentin bonded sticks (0.8 mm(2)). The μTBS of the specimens was tested immediately (IM) or after 6 months of water storage (6M) at 0.5 mm/min. Some sticks at each storage period were immersed in silver nitrate and photo developed, and the NL was evaluated with scanning electron microscopy. Data were analyzed with two-way repeated-measures analysis of variance and Tukey test (α=0.05). At the IM period, PkSe and PkEr showed μTBS similar to the control adhesives (p>0.05) but increased NL pattern and lower μTBS after 6M (p<0.05). ScSe and ScEr showed intermediary μTBS values at the IM period but remained stable after 6 months (p>0.05). AlSe showed the lowest μTBS (p<0.05), but μTBS and NL remained stable after 6M (p>0.05). AlEr showed higher IM μTBS but showed higher degradation after 6M (p<0.05). Universal adhesives that contain MDP showed higher and more stable μTBS with reduced NL at the interfaces after 6 months of water storage.

Structure, morphology, and photoluminescence of porous Si nanowires: effect of different chemical treatments

PubMed Central

2013-01-01

The structure and light-emitting properties of Si nanowires (SiNWs) fabricated by a single-step metal-assisted chemical etching (MACE) process on highly boron-doped Si were investigated after different chemical treatments. The Si nanowires that result from the etching of a highly doped p-type Si wafer by MACE are fully porous, and as a result, they show intense photoluminescence (PL) at room temperature, the characteristics of which depend on the surface passivation of the Si nanocrystals composing the nanowires. SiNWs with a hydrogen-terminated nanostructured surface resulting from a chemical treatment with a hydrofluoric acid (HF) solution show red PL, the maximum of which is blueshifted when the samples are further chemically oxidized in a piranha solution. This blueshift of PL is attributed to localized states at the Si/SiO2 interface at the shell of Si nanocrystals composing the porous SiNWs, which induce an important pinning of the electronic bandgap of the Si material and are involved in the recombination mechanism. After a sequence of HF/piranha/HF treatment, the SiNWs are almost fully dissolved in the chemical solution, which is indicative of their fully porous structure, verified also by transmission electron microscopy investigations. It was also found that a continuous porous Si layer is formed underneath the SiNWs during the MACE process, the thickness of which increases with the increase of etching time. This supports the idea that porous Si formation precedes nanowire formation. The origin of this effect is the increased etching rate at sites with high dopant concentration in the highly doped Si material. PMID:24025542

Effect of fabrication parameters on morphological and optical properties of highly doped p-porous silicon

NASA Astrophysics Data System (ADS)

Zare, Maryam; Shokrollahi, Abbas; Seraji, Faramarz E.

2011-09-01

Porous silicon (PS) layers were fabricated by anodization of low resistive (highly doped) p-type silicon in HF/ethanol solution, by varying current density, etching time and HF concentration. Atomic force microscopy (AFM) and field emission scanning electron microscope (FESEM) analyses were used to investigate the physical properties and reflection spectrum was used to investigate the optical behavior of PS layers in different fabrication conditions. Vertically aligned mesoporous morphology is observed in fabricated films and with HF concentration higher than 20%. The dependence of porosity, layer thickness and rms roughness of the PS layer on current density, etching time and composition of electrolyte is also observed in obtained results. Correlation between reflectivity and fabrication parameters was also explored. Thermal oxidation was performed on some mesoporous layers that resulted in changes of surface roughness, mean height and reflectivity of the layers.

Surface modification of a polyethylene film for anticoagulant and anti-microbial catheter

PubMed Central

Zheng, Yingying; Miao, Jianjun; Zhang, Fuming; Cai, Chao; Koh, Amanda; Simmons, Trevor J.; Mousa, Shaker A.; Linhardt, Robert J.

2016-01-01

A functional anticoagulant and anti-bacterial coating for polyethylene (PE) films is described. The stepwise preparation of this nanocomposite surface coating involves O2 plasma etching of PE film, carbodiimide coupling of cysteamine to the etched PE film, binding of Ag to sulfhydryl groups of cysteamine, and assembly of heparin capped AgNPs on the PE film. The nanocomposite film and its components were characterized by 1H-nuclear magnetic resonance spectroscopy, attenuated total reflectance-Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and field emission-scanning electron microscopy. The resulting PE films demonstrate anticoagulant activity using a hemoglobin whole blood clotting assay, and anti-bacterial activity against Bacillus cereus 3551 (Gram-positive) and Escherichia coli BL21 (Gram-negative) bacteria. The hydrophilicity of the heparin coated PE was determined by contact angle measurements; and the stability of the nanocomposite film, with respect to Ag leaching, was assessed by atomic absorption spectroscopy. PMID:26900340

Preparation of superhydrophobic titanium surfaces via electrochemical etching and fluorosilane modification

NASA Astrophysics Data System (ADS)

Lu, Yao; Xu, Wenji; Song, Jinlong; Liu, Xin; Xing, Yingjie; Sun, Jing

2012-12-01

The preparation of superhydrophobic surfaces on hydrophilic metal substrates depends on both surface microstructures and low surface energy modification. In this study, a simple and inexpensive electrochemical method for preparing robust superhydrophobic titanium surfaces is reported. The neutral sodium chloride solution is used as electrolyte. Fluoroalkylsilane (FAS) was used to reduce the surface energy of the electrochemically etched surface. Scanning electron microscopy (SEM) images, energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) spectra, and contact angle measurement are performed to characterize the morphological features, chemical composition, and wettability of the titanium surfaces. Stability and friction tests indicate that the prepared titanium surfaces are robust. The analysis of electrolyte, reaction process, and products demonstrates that the electrochemical processing is very inexpensive and environment-friendly. This method is believed to be easily adaptable for use in large-scale industry productions to promote the application of superhydrophobic titanium surfaces in aviation, aerospace, shipbuilding, and the military industry.

Sidewall passivation for InGaN/GaN nanopillar light emitting diodes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Choi, Won Hyuck; Abraham, Michael; Yu, Shih-Ying

2014-07-07

We studied the effect of sidewall passivation on InGaN/GaN multiquantum well-based nanopillar light emitting diode (LED) performance. In this research, the effects of varying etch rate, KOH treatment, and sulfur passivation were studied for reducing nanopillar sidewall damage and improving device efficiency. Nanopillars prepared under optimal etching conditions showed higher photoluminescence intensity compared with starting planar epilayers. Furthermore, nanopillar LEDs with and without sulfur passivation were compared through electrical and optical characterization. Suppressed leakage current under reverse bias and four times higher electroluminescence (EL) intensity were observed for passivated nanopillar LEDs compared with unpassivated nanopillar LEDs. The suppressed leakage currentmore » and EL intensity enhancement reflect the reduction of non-radiative recombination at the nanopillar sidewalls. In addition, the effect of sulfur passivation was found to be very stable, and further insight into its mechanism was gained through transmission electron microscopy.« less

Plasma etching of polymers like SU8 and BCB

NASA Astrophysics Data System (ADS)

Mischke, Helge; Gruetzner, Gabi; Shaw, Mark

2003-01-01

Polymers with high viscosity, like SU8 and BCB, play a dominant role in MEMS application. Their behavior in a well defined etching plasma environment in a RIE mode was investigated. The 40.68 MHz driven bottom electrode generates higher etch rates combined with much lower bias voltages by a factor of ten or a higher efficiency of the plasma with lower damaging of the probe material. The goal was to obtain a well-defined process for the removal and structuring of SU8 and BCB using fluorine/oxygen chemistry, defined using variables like electron density and collision rate. The plasma parameters are measured and varied using a production proven technology called SEERS (Self Excited Electron Resonance Spectroscopy). Depending on application and on Polymer several metals are possible (e.g., gold, aluminum). The characteristic of SU8 and BCB was examined in the case of patterning by dry etching in a CF4/O2 chemistry. Etch profile and etch rate correlate surprisingly well with plasma parameters like electron density and electron collision rate, thus allowing to define to adjust etch structure in situ with the help of plasma parameters.

Graphene on silicon dioxide via carbon ion implantation in copper with PMMA-free transfer

NASA Astrophysics Data System (ADS)

Lehnert, Jan; Spemann, Daniel; Hamza Hatahet, M.; Mändl, Stephan; Mensing, Michael; Finzel, Annemarie; Varga, Aron; Rauschenbach, Bernd

2017-06-01

In this work, a synthesis method for the growth of low-defect large-area graphene using carbon ion beam implantation into metallic Cu foils is presented. The Cu foils (1 cm2 in size) were pre-annealed in a vacuum at 950 °C for 2 h, implanted with 35 keV carbon ions at room temperature, and subsequently annealed at 850 °C for 2 h to form graphene layers with the layer number controlled by the implantation fluence. The graphene was then transferred to SiO2/Si substrates by a PMMA-free wet chemical etching process. The obtained regions of monolayer graphene are of ˜900 μm size. Raman spectroscopy, atomic force microscopy, scanning electron microscopy, and optical microscopy performed at room temperature demonstrated a good quality and homogeneity of the graphene layers, especially for monolayer graphene.

Development of scanning graphene Hall probes for magnetic microscopy

NASA Astrophysics Data System (ADS)

Schaefer, Brian T.; Wang, Lei; McEuen, Paul L.; Nowack, Katja C.

We discuss our progress on developing scanning Hall probes fabricated from hexagonal boron nitride (hBN)-encapsulated graphene, with the goal to image magnetic fields with submicron resolution. In contrast to scanning superconducting quantum interference device (SQUID) microscopy, this technique is compatible with a large applied magnetic field and not limited to cryogenic temperatures. The field sensitivity of a Hall probe depends inversely on carrier density, while the primary source of noise in the measurement is Johnson noise originating from the device resistance. hBN-encapsulated graphene demonstrates high carrier mobility at low carrier densities, therefore making it an ideal material for sensitive Hall probes. Furthermore, engineering the dielectric environment of graphene by encapsulating in hBN reduces low-frequency charge noise and disorder from the substrate. We outline our plans for adapting these devices for scanning, including characterization of the point spread function with a scanned current loop and fabrication of a deep-etched structure that enables positioning the sensitive area within 100 nanometers of the sample surface.

Laser-induced phase transitions of Ge2Sb2Te5 thin films used in optical and electronic data storage and in thermal lithography.

PubMed

Chu, Cheng Hung; Shiue, Chiun Da; Cheng, Hsuen Wei; Tseng, Ming Lun; Chiang, Hai-Pang; Mansuripur, Masud; Tsai, Din Ping

2010-08-16

Amorphous thin films of Ge(2)Sb(2)Te(5), sputter-deposited on a ZnS-SiO(2) dielectric layer, are investigated for the purpose of understanding the structural phase-transitions that occur under the influence of tightly-focused laser beams. Selective chemical etching of recorded marks in conjunction with optical, atomic force, and electron microscopy as well as local electron diffraction analysis are used to discern the complex structural features created under a broad range of laser powers and pulse durations. Clarifying the nature of phase transitions associated with laser-recorded marks in chalcogenide Ge(2)Sb(2)Te(5) thin films provides useful information for reversible optical and electronic data storage, as well as for phase-change (thermal) lithography.

Oxide and hydrogen capped ultrasmall blue luminescent Si nanoparticles

NASA Astrophysics Data System (ADS)

Belomoin, Gennadiy; Therrien, Joel; Nayfeh, Munir

2000-08-01

We dispersed electrochemical etched silicon into a colloid of ultrasmall ultrabright Si nanoparticles. Direct imaging using transmission electron microscopy shows particles of ˜1 nm in diameter, and infrared and electron photospectroscopy show that they are passivated with hydrogen. Under 350 nm excitation, the luminescence is dominated by an extremely strong blue band at 390 nm. We replace hydrogen by a high-quality ultrathin surface oxide cap by self-limiting oxidation in H2O2. Upon capping, the excitation efficiency drops, but only by a factor of 2, to an efficiency still two-fold larger than that of fluorescein. Although of slightly lower brightness, capped Si particles have superior biocompatability, an important property for biosensing applications.

Water-assisted growth of graphene on carbon nanotubes by the chemical vapor deposition method.

PubMed

Feng, Jian-Min; Dai, Ye-Jing

2013-05-21

Combining carbon nanotubes (CNTs) with graphene has been proved to be a feasible method for improving the performance of graphene for some practical applications. This paper reports a water-assisted route to grow graphene on CNTs from ferrocene and thiophene dissolved in ethanol by the chemical vapor deposition method in an argon flow. A double injection technique was used to separately inject ethanol solution and water for the preparation of graphene/CNTs. First, CNTs were prepared from ethanol solution and water. The injection of ethanol solution was suspended and water alone was injected into the reactor to etch the CNTs. Thereafter, ethanol solution was injected along with water, which is the key factor in obtaining graphene/CNTs. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and Raman scattering analyses confirmed that the products were the hybrid materials of graphene/CNTs. X-ray photo-electron spectroscopy analysis showed the presence of oxygen rich functional groups on the surface of the graphene/CNTs. Given the activity of the graphene/CNT surface, CdS quantum dots adhered onto it uniformly through simple mechanical mixing.

A structural and electronic comparison of armchair and zigzag epitaxial graphene sidewall nanoribbons

NASA Astrophysics Data System (ADS)

Nevius, Meredith; Wang, F.; Palacio, I.; Celis, A.; Tejeda, A.; Taleb-Ibrahimi, A.; de Heer, W.; Berger, C.; Conrad, E.

2014-03-01

Graphene grown on sidewalls of trenches etched in SiC shows particular promise as a candidate for post-Si CMOS electronics because of its ballistic transport, exceptional mobilities, low intrinsic doping, and the opening of a large band gap. However, before definitive progress can be made toward epitaxial graphene-based transistors, we must fully understand the nuances of graphene ribbon growth on different SiC facets. We have now confirmed that sidewall ribbons grown in graphene's two primary crystallographic directions (``armchair'' and ``zigzag'') differ greatly in both structure and electronic band-structure. We present data from both geometries obtained using low-energy electron microscopy (LEEM), low-energy electron diffraction (LEED), angle-resolved photoemission spectroscopy (ARPES), photoemission electron microscopy (PEEM), micro-ARPES and dark-field micro-ARPES. We demonstrate that while graphene grows on stable facets of trenches oriented for armchair edge growth, trenches oriented for zigzag edge growth prefer narrow ribbons of graphene on the (0001) surface near the trench edge. The structure of these zigzag edge graphene ribbons is complex and paramount to understanding their transport. This work was supported by the NSF under grants DMR-1005880 and DMR-0820382, the W. M. Keck Foundation and the Partner University Fund from the Embassy of France

Coating and functionalization of high density ion track structures by atomic layer deposition

NASA Astrophysics Data System (ADS)

Mättö, Laura; Szilágyi, Imre M.; Laitinen, Mikko; Ritala, Mikko; Leskelä, Markku; Sajavaara, Timo

2016-10-01

In this study flexible TiO2 coated porous Kapton membranes are presented having electron multiplication properties. 800 nm crossing pores were fabricated into 50 μm thick Kapton membranes using ion track technology and chemical etching. Consecutively, 50 nm TiO2 films were deposited into the pores of the Kapton membranes by atomic layer deposition using Ti(iOPr)4 and water as precursors at 250 °C. The TiO2 films and coated membranes were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray reflectometry (XRR). Au metal electrode fabrication onto both sides of the coated foils was achieved by electron beam evaporation. The electron multipliers were obtained by joining two coated membranes separated by a conductive spacer. The results show that electron multiplication can be achieved using ALD-coated flexible ion track polymer foils.

Quantitative biogeography of picoprasinophytes establishes ecotype distributions and significant contributions to marine phytoplankton.

PubMed

Limardo, Alexander J; Sudek, Sebastian; Choi, Chang Jae; Poirier, Camille; Rii, Yoshimi M; Blum, Marguerite; Roth, Robyn; Goodenough, Ursula; Church, Matthew J; Worden, Alexandra Z

2017-08-01

Bathycoccus and Ostreococcus are broadly distributed marine picoprasinophyte algae. We enumerated small phytoplankton using flow cytometry and qPCR assays for phylogenetically distinct Bathycoccus clades BI and BII and Ostreococcus clades OI and OII. Among 259 photic-zone samples from transects and time-series, Ostreococcus maxima occurred in the North Pacific coastal upwelling for OI (36 713 ± 1485 copies ml -1 ) and the Kuroshio Front for OII (50 189 ± 561 copies ml -1 ) and the two overlapped only in frontal regions. The Bathycoccus overlapped more often with maxima along Line-P for BI (10 667 ± 1299 copies ml -1 ) and the tropical Atlantic for BII (4125 ± 339 copies ml -1 ). Only BII and OII were detected at warm oligotrophic sites, accounting for 34 ± 13% of 1589 ± 448 eukaryotic phytoplankton cells ml -1 (annual average) at Station ALOHA's deep chlorophyll maximum. Significant distributional and molecular differences lead us to propose that Bathycoccus clade BII represents a separate species which tolerates higher temperature oceanic conditions than Bathycoccus prasinos (BI). Morphological differences were not evident, but quick-freeze deep-etch electron microscopy provided insight into Bathycoccus scale formation. Our results highlight the importance of quantitative seasonal abundance data for inferring ecological distributions and demonstrate significant, differential picoprasinophyte contributions in mesotrophic and open-ocean waters. © 2017 The Authors. Environmental Microbiology published by Society for Applied Microbiology and John Wiley & Sons Ltd.

Fabrication of a single sub-micron pore spanning a single crystal (100) diamond membrane and impact on particle translocation [Particle translocation through a single crystal diamond pore fabricated by electron beam induced chemical etching

DOE PAGES

Webb, Jennifer R.; Martin, Aiden A.; Johnson, Robert P.; ...

2017-06-21

The fabrication of sub-micron pores in single crystal diamond membranes, which span the entirety of the membrane, is described for the first time, and the translocation properties of polymeric particles through the pore investigated. The pores are produced using a combination of laser micromachining to form the membrane and electron beam induced etching to form the pore. Single crystal diamond as the membrane material, has the advantages of chemical stability and durability, does not hydrate and swell, has outstanding electrical properties that facilitate fast, low noise current-time measurements and is optically transparent for combined optical-conductance sensing. The resulting pores aremore » characterized individually using both conductance measurements, employing a microcapillary electrochemical setup, and electron microscopy. Proof-of-concept experiments to sense charged polystyrene particles as they are electrophoretically driven through a single diamond pore are performed, and the impact of this new pore material on particle translocation is explored. As a result, these findings reveal the potential of diamond as a platform for pore-based sensing technologies and pave the way for the fabrication of single nanopores which span the entirety of a diamond membrane.« less

Fabrication of a single sub-micron pore spanning a single crystal (100) diamond membrane and impact on particle translocation [Particle translocation through a single crystal diamond pore fabricated by electron beam induced chemical etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Webb, Jennifer R.; Martin, Aiden A.; Johnson, Robert P.

The fabrication of sub-micron pores in single crystal diamond membranes, which span the entirety of the membrane, is described for the first time, and the translocation properties of polymeric particles through the pore investigated. The pores are produced using a combination of laser micromachining to form the membrane and electron beam induced etching to form the pore. Single crystal diamond as the membrane material, has the advantages of chemical stability and durability, does not hydrate and swell, has outstanding electrical properties that facilitate fast, low noise current-time measurements and is optically transparent for combined optical-conductance sensing. The resulting pores aremore » characterized individually using both conductance measurements, employing a microcapillary electrochemical setup, and electron microscopy. Proof-of-concept experiments to sense charged polystyrene particles as they are electrophoretically driven through a single diamond pore are performed, and the impact of this new pore material on particle translocation is explored. As a result, these findings reveal the potential of diamond as a platform for pore-based sensing technologies and pave the way for the fabrication of single nanopores which span the entirety of a diamond membrane.« less

Design and fabrication of a large area freestanding compressive stress SiO2 optical window

NASA Astrophysics Data System (ADS)

Van Toan, Nguyen; Sangu, Suguru; Ono, Takahito

2016-07-01

This paper reports the design and fabrication of a 7.2 mm  ×  9.6 mm freestanding compressive stress SiO2 optical window without buckling. An application of the SiO2 optical window with and without liquid penetration has been demonstrated for an optical modulator and its optical characteristic is evaluated by using an image sensor. Two methods for SiO2 optical window fabrication have been presented. The first method is a combination of silicon etching and a thermal oxidation process. Silicon capillaries fabricated by deep reactive ion etching (deep RIE) are completely oxidized to form the SiO2 capillaries. The large compressive stress of the oxide causes buckling of the optical window, which is reduced by optimizing the design of the device structure. A magnetron-type RIE, which is investigated for deep SiO2 etching, is the second method. This method achieves deep SiO2 etching together with smooth surfaces, vertical shapes and a high aspect ratio. Additionally, in order to avoid a wrinkling optical window, the idea of a Peano curve structure has been proposed to achieve a freestanding compressive stress SiO2 optical window. A 7.2 mm  ×  9.6 mm optical window area without buckling integrated with an image sensor for an optical modulator has been successfully fabricated. The qualitative and quantitative evaluations have been performed in cases with and without liquid penetration.

Fabrication of carbon nanowires by pyrolysis of aqueous solution of sugar within asbestos nanofibers

NASA Astrophysics Data System (ADS)

Butko, V. Yu.; Fokin, A. V.; Nevedomskii, V. N.; Kumzerov, Yu. A.

2015-05-01

Carbon nanowires have been fabricated by pyrolysis of an aqueous solution of sugar in nanochannels of asbestos fibers. Electron microscopy demonstrates that the diameter of these nanochannels corresponds to the diameter of the thinnest of the carbon nanowires obtained. Some of these nanowires have a graphite crystal lattice and internal pores. After asbestos is etched out, the carbon nanowires can retain the original shape of the asbestos fibers. Heating in an inert atmosphere reduces the electrical resistivity of the carbon nanowires to ˜0.035 Ω cm.

Cubic GaN quantum dots embedded in zinc-blende AlN microdisks

NASA Astrophysics Data System (ADS)

Bürger, M.; Kemper, R. M.; Bader, C. A.; Ruth, M.; Declair, S.; Meier, C.; Förstner, J.; As, D. J.

2013-09-01

Microresonators containing quantum dots find application in devices like single photon emitters for quantum information technology as well as low threshold laser devices. We demonstrate the fabrication of 60 nm thin zinc-blende AlN microdisks including cubic GaN quantum dots using dry chemical etching techniques. Scanning electron microscopy analysis reveals the morphology with smooth surfaces of the microdisks. Micro-photoluminescence measurements exhibit optically active quantum dots. Furthermore this is the first report of resonator modes in the emission spectrum of a cubic AlN microdisk.

Facile Fabrication of Uniform Polyaniline Nanotubes with Tubular Aluminosilicates as Templates

PubMed Central

2008-01-01

The uniform polyaniline (PANI) nanotubes, with inner diameter, outer diameter, and tubular thickness of 40, 60, and 10 nm, respectively, were prepared successfully by using natural tubular aluminosilicates as templates. The halloysite nanotubes were coated with PANI via the in situ chemical oxidation polymerization. Then the templates were etched with HCl/HF solution. The PANI nanotubes were characterized using FTIR, X-ray diffraction, and transmission electron microscopy. The conductivity of the PANI nanotubes was found to be 1.752 × 10−5(Ω·cm)−1.

Facile Fabrication of Uniform Polyaniline Nanotubes with Tubular Aluminosilicates as Templates

NASA Astrophysics Data System (ADS)

Zhang, Long; Liu, Peng

2008-08-01

The uniform polyaniline (PANI) nanotubes, with inner diameter, outer diameter, and tubular thickness of 40, 60, and 10 nm, respectively, were prepared successfully by using natural tubular aluminosilicates as templates. The halloysite nanotubes were coated with PANI via the in situ chemical oxidation polymerization. Then the templates were etched with HCl/HF solution. The PANI nanotubes were characterized using FTIR, X-ray diffraction, and transmission electron microscopy. The conductivity of the PANI nanotubes was found to be 1.752 × 10-5 (Ω·cm)-1.

Influence of surface pre-treatment on the electronic levels in silicon MaWCE nanowires.

PubMed

Venturi, Giulia; Castaldini, Antonio; Schleusener, Alexander; Sivakov, Vladimir; Cavallini, Anna

2015-05-15

Deep level transient spectroscopy (DLTS) was performed on n-doped silicon nanowires grown by metal-assisted wet chemical etching (MaWCE) with gold as the catalyst in order to investigate the energetic scheme inside the bandgap. To observe the possible dependence of the level scheme on the processing temperature, DLTS measurements were performed on the nanowires grown on a non-treated Au/Si surface and on a thermally pre-treated Au/Si surface. A noticeable modification of the configuration of the energy levels was observed, induced by the annealing process. Based on our results on these MaWCE nanowires and on literature data about deep levels in bulk silicon, some hypotheses were advanced regarding the identification of the defects responsible of the energy levels revealed.

Fast synthesis of porous NiCo2O4 hollow nanospheres for a high-sensitivity non-enzymatic glucose sensor

NASA Astrophysics Data System (ADS)

Huang, Wei; Cao, Yang; Chen, Yong; Peng, Juan; Lai, Xiaoyong; Tu, Jinchun

2017-02-01

In this paper, we report the fast synthesis of porous NiCo2O4 hollow nanospheres via a polycrystalline Cu2O-templated route based on the elaborately designed "coordinating etching and precipitating" process. The composition and morphology of the porous NiCo2O4 hollow nanospheres were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy. The electron-transfer capability and electrocatalytic activity of the materials were investigated by electrochemical impedance spectroscopy and cyclic voltammetry. NiCo2O4 was endowed with superior electron-transfer capability, large surface area, and abundant intrinsic redox couples of Ni2+/Ni3+ and Co2+/Co3+ ions; thus, the modified electrode exhibited excellent glucose-sensing properties, with a high sensitivity of 1917 μA·mM-1·cm-2 at a low concentration, a good linear range from 0.01 mM to 0.30 mM and from 0.30 mM to 2.24 mM, and a low detection limit of 0.6 μM (S/N = 3).

Deep-branching Novel Lineages and High Diversity of Haptophytes in the Skagerrak (Norway) Uncovered by 454 Pyrosequencing

PubMed Central

Egge, Elianne S; Eikrem, Wenche; Edvardsen, Bente

2015-01-01

Microalgae in the division Haptophyta may be difficult to identify to species by microscopy because they are small and fragile. Here, we used high-throughput sequencing to explore the diversity of haptophytes in outer Oslofjorden, Skagerrak, and supplemented this with electron microscopy. Nano- and picoplanktonic subsurface samples were collected monthly for 2 yr, and the haptophytes were targeted by amplification of RNA/cDNA with Haptophyta-specific 18S ribosomal DNA V4 primers. Pyrosequencing revealed higher species richness of haptophytes than previously observed in the Skagerrak by microscopy. From ca. 400,000 reads we obtained 156 haptophyte operational taxonomic units (OTUs) after rigorous filtering and 99.5% clustering. The majority (84%) of the OTUs matched environmental sequences not linked to a morphological species, most of which were affiliated with the order Prymnesiales. Phylogenetic analyses including Oslofjorden OTUs and available cultured and environmental haptophyte sequences showed that several of the OTUs matched sequences forming deep-branching lineages, potentially representing novel haptophyte classes. Pyrosequencing also retrieved cultured species not previously reported by microscopy in the Skagerrak. Electron microscopy revealed species not yet genetically characterised and some potentially novel taxa. This study contributes to linking genotype to phenotype within this ubiquitous and ecologically important protist group, and reveals great, unknown diversity. PMID:25099994

Effects of epitaxial structure and processing on electrical characteristics of InAs-based nBn infrared detectors

NASA Astrophysics Data System (ADS)

Du, X.; Savich, G. R.; Marozas, B. T.; Wicks, G. W.

2017-02-01

The conventional processing of the III-V nBn photodetectors defines mesa devices by etching the contact n-layer and stopping immediately above the barrier, i.e., a shallow etch. This processing enables great suppression of surface leakage currents without having to explore surface passivation techniques. However, devices that are made with this processing scheme are subject to lateral diffusion currents. To address the lateral diffusion current, we compare the effects of different processing approaches and epitaxial structures of nBn detectors. The conventional solution for eliminating lateral diffusion current, a deep etch through the barrier and the absorber, creates increased dark currents and an increased device failure rate. To avoid deep etch processing, a new device structure is proposed, the inverted-nBn structure. By comparing with the conventional nBn structure, the results show that the lateral diffusion current is effectively eliminated in the inverted-nBn structure without elevating the dark currents.

Characterization of nanostructured CuO-porous silicon matrix formed on copper-coated silicon substrate via electrochemical etching

NASA Astrophysics Data System (ADS)

Naddaf, M.; Mrad, O.; Al-zier, A.

2014-06-01

A pulsed anodic etching method has been utilized for nanostructuring of a copper-coated p-type (100) silicon substrate, using HF-based solution as electrolyte. Scanning electron microscopy reveals the formation of a nanostructured matrix that consists of island-like textures with nanosize grains grown onto fiber-like columnar structures separated with etch pits of grooved porous structures. Spatial micro-Raman scattering analysis indicates that the island-like texture is composed of single-phase cupric oxide (CuO) nanocrystals, while the grooved porous structure is barely related to formation of porous silicon (PS). X-ray diffraction shows that both the grown CuO nanostructures and the etched silicon layer have the same preferred (220) orientation. Chemical composition obtained by means of X-ray photoelectron spectroscopic (XPS) analysis confirms the presence of the single-phase CuO on the surface of the patterned CuO-PS matrix. As compared to PS formed on the bare silicon substrate, the room-temperature photoluminescence (PL) from the CuO-PS matrix exhibits an additional weak `blue' PL band as well as a blue shift in the PL band of PS (S-band). This has been revealed from XPS analysis to be associated with the enhancement in the SiO2 content as well as formation of the carbonyl group on the surface in the case of the CuO-PS matrix.

Imaging resin infiltration into non-cavitated carious lesions by optical coherence tomography.

PubMed

Schneider, Hartmut; Park, Kyung-Jin; Rueger, Claudia; Ziebolz, Dirk; Krause, Felix; Haak, Rainer

2017-05-01

Visualisation of the etching process and resin penetration at white spot carious lesions by spectral domain optical coherence tomography (SD-OCT). The non-cavitated carious lesions (ICDAS code 2) of four visually preselected extracted human molars and premolars were verified as enamel lesions by micro computed tomography (μCT). One region of interest (ROI) per tooth was marked by two drill-holes in occlusal-cervical direction. The lesions were imaged by SD-OCT. Lesions were infiltrated (Icon, DMG) according to the manufacturer's instructions. During each treatment step and after light curing of the infiltrant, the ROIs were imaged again by SD-OCT. Teeth were sectioned through the ROIs and section layers were imaged by scanning electron microscopy in order to compare with the OCT images. The image sequences for etching and infiltration were viewed in time lapse. During the etching process, numerous bubbles formed on the lesion surface. Using OCT, the process of resin penetration into the carious lesion body became visible. The early enamel carious lesion was completely infiltrated by the resin whereas infiltration of the advanced enamel carious lesion was incomplete and inhomogeneous. Resin infiltration can be increased by optimizing the etching process. Optical coherence tomography provides information about the process and degree of resin infiltration. Active acid application before resin infiltration is recommendable. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fabrication of vertical nanowire resonators for aerosol exposure assessment

NASA Astrophysics Data System (ADS)

Merzsch, Stephan; Wasisto, Hutomo Suryo; Stranz, Andrej; Hinze, Peter; Weimann, Thomas; Peiner, Erwin; Waag, Andreas

2013-05-01

Vertical silicon nanowire (SiNW) resonators are designed and fabricated in order to assess exposure to aerosol nanoparticles (NPs). To realize SiNW arrays, nanolithography and inductively coupled plasma (ICP) deep reactive ion etching (DRIE) at cryogenic temperature are utilized in a top-down fabrication of SiNW arrays which have high aspect ratios (i.e., up to 34). For nanolithography process, a resist film thickness of 350 nm is applied in a vacuum contact mode to serve as a mask. A pattern including various diameters and distances for creating pillars is used (i.e., 400 nm up to 5 μm). In dry etching process, the etch rate is set high of 1.5 μm/min to avoid underetching. The etch profiles of Si wires can be controlled aiming to have either perpendicularly, negatively or positively profiled sidewalls by adjusting the etching parameters (e.g., temperature and oxygen content). Moreover, to further miniaturize the wire, multiple sacrificial thermal oxidations and subsequent oxide stripping are used yielding SiNW arrays of 650 nm in diameter and 40 μm in length. In the resonant frequency test, a piezoelectric shear actuator is integrated with the SiNWs inside a scanning electron microscope (SEM) chamber. The observation of the SiNW deflections are performed and viewed from the topside of the SiNWs to reduce the measurement redundancy. Having a high deflection of ~10 μm during its resonant frequency of 452 kHz and a low mass of 31 pg, the proposed SiNW is potential for assisting the development of a portable aerosol resonant sensor.

From Spintronics to CFD/ContractForDifferences

NASA Astrophysics Data System (ADS)

Maksoed, W. H.

2015-11-01

Involve the CFD/Computational Fluid Dynamics & HCCI/Homogeneous Charge Compression Ignition - Marcine Frackowiak, dissertation, 2009, for CFD/Contract For Differences accompanied by ``One Man's Crusade to Exonerate Hydrogen for Hindenburg Disaster'' of Addison BAIN, APS News, v. 9, n.7 (July 2000) concludes ``ignition of the blaze'' are responsible to those May, 1937 Accidents. Spintronics their selves include active control & manipulation of spin degree of freedom ever denotes: the nano-obelisk of scanning electron microscopy of galliumnitride/GaN nanostructures-Yong-Hon Cho et al.:``Novel Photonic Device using core-shell nanostructures'', SPIE-newsroom,10.1117/2.1201503.005864. Herewith commercial activated carbon/C can be imaged directly using abberation-corrected transmission electron microscopy[PJF Harris et al.: ``Imaging the Atomic Structures of activated C'', J. Phys. Condens. Matt, 20 (2008) in fig b & c- images networks of hexagonal rings can be clearly be seen depicts equal etchings of 340 px Akhenaten, Nefertiti & their childrens. Incredible acknowledgments to Minister of Education & Culture RI 1998-1999 HE. Mr. Prof. Ir. WIRANTO ARISMUNANDAR, MSME.

Nitridation of porous GaAs by an ECR ammonia plasma

NASA Astrophysics Data System (ADS)

Naddaf, M.; Hullavarad, S. S.; Ganesan, V.; Bhoraskar, S. V.

2006-02-01

The effect of surface porosity of GaAs on the nature of growth of GaN, by use of plasma nitridation of GaAs, has been investigated. Porous GaAs samples were prepared by anodic etching of n-type (110) GaAs wafers in HCl solution. Nitridation of porous GaAs samples were carried out by using an electron-cyclotron resonance-induced ammonia plasma. The formation of mixed phases of GaN was investigated using the grazing angle x-ray diffraction method. A remarkable improvement in the intensity of photoluminescence (PL) compared with that of GaN synthesized by direct nitriding of GaAs surface has been observed. The PL intensity of nitrided porous GaAs at the temperature of 380 °C was found to be about two orders of magnitude higher as compared with the directly nitrided GaAs at the temperature of 500 °C. The changes in the morphology of nitrided porous GaAs have been investigated using both scanning electron microscopy and atomic force microscopy.

A feasible method to eliminate nanoleakage in dentin hybrid layers.

PubMed

Chen, Ji-Hua; Liu, Yan; Niu, Li-Na; Lu, Shuai; Tay, Franklin R; Gao, Yu

2014-10-01

To determine whether high-pressure air blowing during adhesive application affects the infiltration of resin comonomers and nanoleakage manifestation in the resin/dentin interface under simulated pulpal pressure. Thirty mid-coronal dentin surfaces were bonded with an etch-and-rinse adhesive (Adper Single Bond 2) under simulated pulpal pressure. In the control group, the adhesive was thinned by ordinary air blowing with a pressure of 0.2 MPa, while in the experimental group, a high-pressure air blowing technique (pressure: 0.4 MPa) was used. All other procedures followed the manufacturer's instructions. Resin tag formation and nanoleakage in the bonding interface were evaluated with scanning electron microscopy (SEM) and transmission electron microscopy (TEM). When adhesive was thinned with high pressure air blowing, longer and more homogeneous resin tags were formed. The bonding interface demonstrated good overall morphology and integrity. Almost perfect infiltration of resin and no obvious nanoleakage were observed. Thinning of adhesive with high-pressure air blowing provides a clinically feasible adjunctive procedure for better resin infiltration.

Bulk and Surface Morphologies of ABC Miktoarm Star Terpolymers Composed of PDMS, PI, and PMMA Arms

DOE PAGES

Chernyy, Sergey; Kirkensgaard, Jacob Judas Kain; Mahalik, Jyoti P.; ...

2018-02-02

DIM miktoarm star copolymers, composed of polydimethylsiloxane [D], poly(1,4-isoprene) [I], and poly(methyl methacrylate) [M], were synthesized using a newly developed linking methodology with 4-allyl-1,1-diphenylethylene as a linking agent. The equilibrium bulk morphologies of the DIM stars were found to range from [6.6.6] tiling patterns to alternating lamellar and alternating cylindrical morphologies, as determined experimentally by small-angle X-ray scattering and transmission electron microscopy and confirmed by dissipative particle dynamics and self-consistent field theory based arguments. The thin film morphologies, which differ from those found in the bulk, were identified by scanning electron microscopy, coupled with oxygen plasma etching. Finally, square arraysmore » of the PDMS nanodots and empty core cylinders were formed on silica after oxygen plasma removal of the poly(1,4-isoprene) and poly(methyl methacrylate) which generated nanostructured substrates decorated with these features readily observable.« less

Bulk and Surface Morphologies of ABC Miktoarm Star Terpolymers Composed of PDMS, PI, and PMMA Arms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chernyy, Sergey; Kirkensgaard, Jacob Judas Kain; Mahalik, Jyoti P.

DIM miktoarm star copolymers, composed of polydimethylsiloxane [D], poly(1,4-isoprene) [I], and poly(methyl methacrylate) [M], were synthesized using a newly developed linking methodology with 4-allyl-1,1-diphenylethylene as a linking agent. The equilibrium bulk morphologies of the DIM stars were found to range from [6.6.6] tiling patterns to alternating lamellar and alternating cylindrical morphologies, as determined experimentally by small-angle X-ray scattering and transmission electron microscopy and confirmed by dissipative particle dynamics and self-consistent field theory based arguments. The thin film morphologies, which differ from those found in the bulk, were identified by scanning electron microscopy, coupled with oxygen plasma etching. Finally, square arraysmore » of the PDMS nanodots and empty core cylinders were formed on silica after oxygen plasma removal of the poly(1,4-isoprene) and poly(methyl methacrylate) which generated nanostructured substrates decorated with these features readily observable.« less

Self-assembled molecular magnets on patterned silicon substrates: bridging bio-molecules with nanoelectronics.

PubMed

Chang, Chia-Ching; Sun, Kien Wen; Lee, Shang-Fan; Kan, Lou-Sing

2007-04-01

The paper reports the methods of preparing molecular magnets and patterning of the molecules on a semiconductor surface. A highly magnetically aligned metallothionein containing Mn and Cd (Mn,Cd-MT-2) is first synthesized, and the molecules are then placed into nanopores prepared on silicon (001) surfaces using electron beam lithography and reactive ion-etching techniques. We have observed the self-assemble growth of the MT molecules on the patterned Si surface such that the MT molecules have grown into rod or ring type three-dimensional nanostructures, depending on the patterned nanostructures on the surface. We also provide scanning electron microscopy, atomic force microscopy, and magnetic force microscope studies of the molecular nanostructures. This engineered molecule shows molecular magnetization and is biocompatible with conventional semiconductors. These features make Mn,Cd-MT-2 a good candidate for biological applications and sensing sources of new nanodevices. Using molecular self-assembly and topographical patterning of the semiconductor substrate, we can close the gap between bio-molecules and nanoelectronics built into the semiconductor chip.

Dynamic Pattern Formation in Electron-Beam-Induced Etching [Emergent formation of dynamic topographic patterns in electron beam induced etching

DOE PAGES

Martin, Aiden A.; Bahm, Alan; Bishop, James; ...

2015-12-15

Here, we report highly ordered topographic patterns that form on the surface of diamond, span multiple length scales, and have a symmetry controlled by the precursor gas species used in electron-beam-induced etching (EBIE). The pattern formation dynamics reveals an etch rate anisotropy and an electron energy transfer pathway that is overlooked by existing EBIE models. Therefore, we, modify established theory such that it explains our results and remains universally applicable to EBIE. Furthermore, the patterns can be exploited in controlled wetting, optical structuring, and other emerging applications that require nano- and microscale surface texturing of a wide band-gap material.

Silicon etching of difluoromethane atmospheric pressure plasma jet combined with its spectroscopic analysis

NASA Astrophysics Data System (ADS)

Sung, Yu-Ching; Wei, Ta-Chin; Liu, You-Chia; Huang, Chun

2018-06-01

A capacitivly coupled radio-frequency double-pipe atmospheric-pressure plasma jet is used for etching. An argon carrier gas is supplied to the plasma discharge jet; and CH2F2 etch gas is inserted into the plasma discharge jet, near the silicon substrate. Silicon etchings rate can be efficiently-controlled by adjusting the feeding etching gas composition and plasma jet operating parameters. The features of silicon etched by the plasma discharge jet are discussed in order to spatially spreading plasma species. Electronic excitation temperature and electron density are detected by increasing plasma power. The etched silicon profile exhibited an anisotropic shape and the etching rate was maximum at the total gas flow rate of 4500 sccm and CH2F2 concentration of 11.1%. An etching rate of 17 µm/min was obtained at a plasma power of 100 W.

III-Nitride Blue Laser Diode with Photoelectrochemically Etched Current Aperture

NASA Astrophysics Data System (ADS)

Megalini, Ludovico

Group III-nitride is a remarkable material system to make highly efficient and high-power optoelectronics and electronic devices because of the unique electrical, physical, chemical and structural properties it offers. In particular, InGaN-based blue Laser Diodes (LDs) have been successfully employed in a variety of applications ranging from biomedical and military devices to scientific instrumentation and consumer electronics. Recently their use in highly efficient Solid State Lighting (SSL) has been proposed because of their superior beam quality and higher efficiency at high input power density. Tremendous advances in research of GaN semi-polar and non-polar crystallographic planes have led both LEDs and LDs grown on these non-basal planes to rival with, and with the promise to outperform, their equivalent c-plane counterparts. However, still many issues need to be addressed, both related to material growth and device fabrication, including a lack of conventional wet etching techniques. GaN and its alloys with InN and AlN have proven resistant essentially to all known standard wet etching techniques, and the predominant etching methods rely on chlorine-based dry etching (RIE). These introduce sub-surface damage which can degrade the electrical properties of the epitaxial structure and reduce the reliability and lifetime of the final device. Such reasons and the limited effectiveness of passivation techniques have so far suggested to etch the LD ridges before the active region, although it is well-known that this can badly affect the device performance, especially in narrow stripe width LDs, because the gain guiding obtained in the planar configuration is weak and the low index step and high lateral current leakage result in devices with threshold current density higher than devices whose ridge is etched beyond the active region. Moreover, undercut etching of III-nitride layers has proven even more challenging, with limitations in control of the lateral etch distance. In this dissertation it is presented the first nitride blue edge emitting LD with a photoelectrochemical etched current aperture (CA-LD) into the device active region. Photoelectrochemical etching (PECE) has emerged as a powerful wet etching technique for III-nitride compounds. Beyond the advantages of wet etching technique, PECE offers bandgap selectivity, which is particularly desirable because it allows more freedom in designing new and advanced devices with higher performances. In the first part of this thesis a review of PECE is presented, and it is shown how it can be used to achieve a selective and controllable deep undercut of the active region of LEDs and LDs, in particular the selective PECE of MQW active region of (10-10) m-plane and (20-2-1) plane structures is reported. In the second part of this thesis, the fabrication flow process of the CA-LD is described. The performance of these devices is compared with that of shallow etched ridge LDs with a nominally identical epitaxial structure and active region width and it is experimentally shown that the CA-LD design has superior performance. CW operation of a (20-2-1) CA-LD with a 1.5 microm wide active region is demonstrated. Finally, in the third and last part of this thesis, the CA-LD performance is discussed in more details, in particular, an analysis of optical scattering losses caused by the rough edges of the remnant PEC etched active region is presented.

Note: Circuit design for direct current and alternating current electrochemical etching of scanning probe microscopy tips.

PubMed

Jobbins, Matthew M; Raigoza, Annette F; Kandel, S Alex

2012-03-01

We present control circuits designed for electrochemically etching, reproducibly sharp STM probes. The design uses an Arduino UNO microcontroller to allow for both ac and dc operation, as well as a comparator driven shut-off that allows for etching to be stopped in 0.5-1 μs. The Arduino allows the instrument to be customized to suit a wide variety of potential applications without significant changes to hardware. Data is presented for coarse chemical etching of 80:20 platinum-iridium, tungsten, and nickel tips.

Observation of thermally etched grain boundaries with the FIB/TEM technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Palizdar, Y., E-mail: y.palizdar@merc.ac.ir; San Martin, D.; Ward, M.

2013-10-15

Thermal etching is a method which is able to reveal and characterize grain boundaries, twins or dislocation structures and determine parameters such as grain boundary energies, surface diffusivities or study phase transformations in steels, intermetallics or ceramic materials. This method relies on the preferential transfer of matter away from grain boundaries on a polished sample during heating at high temperatures in an inert/vacuum atmosphere. The evaporation/diffusion of atoms at high temperatures results in the formation of grooves at the intersections of the planes of grain/twin boundaries with the polished surface. This work describes how the combined use of Focussed Ionmore » Beam and Transmission Electron Microscopy can be used to characterize not only the grooves and their profile with the surface, but also the grain boundary line below the groove, this method being complementary to the commonly used scanning probe techniques. - Highlights: • Thermally etched low-carbon steel samples have been characterized by FIB/TEM • Grain boundary (GB) lines below the groove have been characterized in this way • Absence of ghost traces and large θ angle suggests that GB are not stationary but mobile • Observations correlate well with previous works and Mullins' investigations [22].« less

Fabrication of Meso-Porous Sintered Metal Thin Films by Selective Etching of Silica Based Sacrificial Template

PubMed Central

Dumée, Ludovic F.; She, Fenghua; Duke, Mikel; Gray, Stephen; Hodgson, Peter; Kong, Lingxue

2014-01-01

Meso-porous metal materials have enhanced surface energies offering unique surface properties with potential applications in chemical catalysis, molecular sensing and selective separation. In this paper, commercial 20 nm diameter metal nano-particles, including silver and copper were blended with 7 nm silica nano-particles by shear mixing. The resulted powders were cold-sintered to form dense, hybrid thin films. The sacrificial silica template was then removed by selective etching in 12 wt% hydrofluoric acid solutions for 15 min to reveal a purely metallic meso-porous thin film material. The impact of the initial silica nano-particle diameter (7–20 nm) as well as the sintering pressure (5–20 ton·m−2) and etching conditions on the morphology and properties of the final nano-porous thin films were investigated by porometry, pyknometery, gas and liquid permeation and electron microscopy. Furthermore, the morphology of the pores and particle aggregation during shear mixing were assessed through cross-sectioning by focus ion beam milling. It is demonstrated that meso-pores ranging between 50 and 320 nm in average diameter and porosities up to 47% can be successfully formed for the range of materials tested. PMID:28344241

In situ photoacoustic characterization for porous silicon growing: Detection principles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ramirez-Gutierrez, C. F.; Licenciatura en Ingeniería Física, Facultad de Ingeniería, Universidad Autónoma de Querétaro, C. P. 76010 Querétaro, Qro.; Castaño-Yepes, J. D.

There are a few methodologies for monitoring the in-situ formation of Porous Silicon (PS). One of the methodologies is photoacoustic. Previous works that reported the use of photoacoustic to study the PS formation do not provide the physical explanation of the origin of the signal. In this paper, a physical explanation of the origin of the photoacoustic signal during the PS etching is provided. The incident modulated radiation and changes in the reflectance are taken as thermal sources. In this paper, a useful methodology is proposed to determine the etching rate, porosity, and refractive index of a PS film bymore » the determination of the sample thickness, using scanning electron microscopy images. This method was developed by carrying out two different experiments using the same anodization conditions. The first experiment consisted of growth of the samples with different etching times to prove the periodicity of the photoacoustic signal, while the second one considered the growth samples using three different wavelengths that are correlated with the period of the photoacoustic signal. The last experiment showed that the period of the photoacoustic signal is proportional to the laser wavelength.« less

Deterministic Nanopatterning of Diamond Using Electron Beams.

PubMed

Bishop, James; Fronzi, Marco; Elbadawi, Christopher; Nikam, Vikram; Pritchard, Joshua; Fröch, Johannes E; Duong, Ngoc My Hanh; Ford, Michael J; Aharonovich, Igor; Lobo, Charlene J; Toth, Milos

2018-03-27

Diamond is an ideal material for a broad range of current and emerging applications in tribology, quantum photonics, high-power electronics, and sensing. However, top-down processing is very challenging due to its extreme chemical and physical properties. Gas-mediated electron beam-induced etching (EBIE) has recently emerged as a minimally invasive, facile means to dry etch and pattern diamond at the nanoscale using oxidizing precursor gases such as O 2 and H 2 O. Here we explain the roles of oxygen and hydrogen in the etch process and show that oxygen gives rise to rapid, isotropic etching, while the addition of hydrogen gives rise to anisotropic etching and the formation of topographic surface patterns. We identify the etch reaction pathways and show that the anisotropy is caused by preferential passivation of specific crystal planes. The anisotropy can be controlled by the partial pressure of hydrogen and by using a remote RF plasma source to radicalize the precursor gas. It can be used to manipulate the geometries of topographic surface patterns as well as nano- and microstructures fabricated by EBIE. Our findings constitute a comprehensive explanation of the anisotropic etch process and advance present understanding of electron-surface interactions.

Cryogenic Etching of High Aspect Ratio 400 nm Pitch Silicon Gratings.

PubMed

Miao, Houxun; Chen, Lei; Mirzaeimoghri, Mona; Kasica, Richard; Wen, Han

2016-10-01

The cryogenic process and Bosch process are two widely used processes for reactive ion etching of high aspect ratio silicon structures. This paper focuses on the cryogenic deep etching of 400 nm pitch silicon gratings with various etching mask materials including polymer, Cr, SiO 2 and Cr-on-polymer. The undercut is found to be the key factor limiting the achievable aspect ratio for the direct hard masks of Cr and SiO 2 , while the etch selectivity responds to the limitation of the polymer mask. The Cr-on-polymer mask provides the same high selectivity as Cr and reduces the excessive undercut introduced by direct hard masks. By optimizing the etching parameters, we etched a 400 nm pitch grating to ≈ 10.6 μ m depth, corresponding to an aspect ratio of ≈ 53.

Specimen preparation by ion beam slope cutting for characterization of ductile damage by scanning electron microscopy.

PubMed

Besserer, Hans-Bernward; Gerstein, Gregory; Maier, Hans Jürgen; Nürnberger, Florian

2016-04-01

To investigate ductile damage in parts made by cold sheet-bulk metal forming a suited specimen preparation is required to observe the microstructure and defects such as voids by electron microscopy. By means of ion beam slope cutting both a targeted material removal can be applied and mechanical or thermal influences during preparation avoided. In combination with scanning electron microscopy this method allows to examine voids in the submicron range and thus to analyze early stages of ductile damage. In addition, a relief structure is formed by the selectivity of the ion bombardment, which depends on grain orientation and microstructural defects. The formation of these relief structures is studied using scanning electron microscopy and electron backscatter diffraction and the use of this side effect to interpret the microstructural mechanisms of voids formation by plastic deformation is discussed. A comprehensive investigation of the suitability of ion beam milling to analyze ductile damage is given at the examples of a ferritic deep drawing steel and a dual phase steel. © 2016 Wiley Periodicals, Inc.

Etch pit investigation of free electron concentration controlled 4H-SiC

NASA Astrophysics Data System (ADS)

Kim, Hong-Yeol; Shin, Yun Ji; Kim, Jung Gon; Harima, Hiroshi; Kim, Jihyun; Bahng, Wook

2013-04-01

Etch pits were investigated using the molten KOH selective etching method to examine dependence of etch pit shape and size on free electron concentration. The free electron concentrations of highly doped 4H-silicon carbide (SiC) were controlled by proton irradiation and thermal annealing, which was confirmed by a frequency shift in the LO-phonon-plasmon-coupled (LOPC) mode on micro-Raman spectroscopy. The proton irradiated sample with 5×1015 cm-2 fluence and an intrinsic semi-insulating sample showed clearly classified etch pits but different ratios of threading screw dislocation (TSD) and threading edge dislocation (TED) sizes. Easily classified TEDs and TSDs on proton irradiated 4H-SiC were restored as highly doped 4H-SiC after thermal annealing due to the recovered carrier concentrations. The etched surface of proton irradiated 4H-SiC and boron implanted SiC showed different surface conditions after activation.

Atomic precision etch using a low-electron temperature plasma

NASA Astrophysics Data System (ADS)

Dorf, L.; Wang, J.-C.; Rauf, S.; Zhang, Y.; Agarwal, A.; Kenney, J.; Ramaswamy, K.; Collins, K.

2016-03-01

Sub-nm precision is increasingly being required of many critical plasma etching processes in the semiconductor industry. Accurate control over ion energy and ion/radical composition is needed during plasma processing to meet these stringent requirements. Described in this work is a new plasma etch system which has been designed with the requirements of atomic precision plasma processing in mind. In this system, an electron sheet beam parallel to the substrate surface produces a plasma with an order of magnitude lower electron temperature Te (~ 0.3 eV) and ion energy Ei (< 3 eV without applied bias) compared to conventional radio-frequency (RF) plasma technologies. Electron beam plasmas are characterized by higher ion-to-radical fraction compared to RF plasmas, so a separate radical source is used to provide accurate control over relative ion and radical concentrations. Another important element in this plasma system is low frequency RF bias capability which allows control of ion energy in the 2-50 eV range. Presented in this work are the results of etching of a variety of materials and structures performed in this system. In addition to high selectivity and low controllable etch rate, an important requirement of atomic precision etch processes is no (or minimal) damage to the remaining material surface. It has traditionally not been possible to avoid damage in RF plasma processing systems, even during atomic layer etch. The experiments for Si etch in Cl2 based plasmas in the aforementioned etch system show that damage can be minimized if the ion energy is kept below 10 eV. Layer-by-layer etch of Si is also demonstrated in this etch system using electrical and gas pulsing.

Development of a DNA Sensor Based on Nanoporous Pt-Rich Electrodes

NASA Astrophysics Data System (ADS)

Van Hao, Pham; Thanh, Pham Duc; Xuan, Chu Thi; Hai, Nguyen Hoang; Tuan, Mai Anh

2017-06-01

Nanoporous Pt-rich electrodes with 72 at.% Pt composition were fabricated by sputtering a Pt-Ag alloy, followed by an electrochemical dealloying process to selectively etch away Ag atoms. The surface properties of nanoporous membranes were investigated by energy-dispersive x-ray spectroscopy (EDS), scanning electron microscopy (SEM), atomic force microscopy (AFM), a documentation system, and a gel image system (Gel Doc Imager). A single strand of probe deoxyribonucleic acid (DNA) was immobilized onto the electrode surface by physical adsorption. The DNA probe and target hybridization were measured using a lock-in amplifier and an electrochemical impedance spectroscope (EIS). The nanoporous Pt-rich electrode-based DNA sensor offers a fast response time of 3.7 s, with a limit of detection (LOD) of 4.35 × 10-10 M of DNA target.

Layer-controllable graphene by plasma thinning and post-annealing

NASA Astrophysics Data System (ADS)

Zhang, Lufang; Feng, Shaopeng; Xiao, Shaoqing; Shen, Gang; Zhang, Xiumei; Nan, Haiyan; Gu, Xiaofeng; Ostrikov, Kostya (Ken)

2018-05-01

The electronic structure of graphene depends crucially on its layer number and therefore engineering the number of graphene's atomic stacking layers is of great importance for the preparation of graphene-based devices. In this paper, we demonstrated a relatively less invasive, high-throughput and uniform large-area plasma thinning of graphene based on direct bombardment effect of fast-moving ionic hydrogen or argon species. Any desired number of graphene layers including trilayer, bilayer and monolayer can be obtained. Structural changes of graphene layers are studied by optical microscopy, Raman spectroscopy and atomic force microscopy. Post annealing is adopted to self-heal the lattice defects induced by the ion bombardment effect. This plasma etching technique is efficient and compatible with semiconductor manufacturing processes, and may find important applications for graphene-based device fabrication.

Development of refractive X-ray focusing optics at Diamond Light Source

NASA Astrophysics Data System (ADS)

Alianelli, L.; Sawhney, K. J. S.; Loader, I. M.; Jenkins, D. W. K.; Stevens, R.; Snigirev, A.; Snigireva, I.

2007-09-01

The Diamond Optics & Metrology Group and the collaborators at the STFC Central Microstructure Facility have initiated a program for the design and fabrication of in-line micro- and nano-focusing optics for synchrotron radiation beamlines. The first type of optics fabricated is a kinoform lens in silicon on the same model proposed by K. Evans- Lutterodt et al [Opt. Expr. 11 (2003) 919.]. The fabrication utilised ultra high resolution electron beam lithographic patterning of an electron sensitive SU8 polymer and deep reactive ion etching of silicon. The first test of the focusing properties was performed at the ESRF BM5 optics beamline. In this paper we present details on the design and fabrication, and discuss the test results.

Redox responsive nanotubes from organometallic polymers by template assisted layer by layer fabrication

NASA Astrophysics Data System (ADS)

Song, Jing; Jańczewski, Dominik; Guo, Yuanyuan; Xu, Jianwei; Vancso, G. Julius

2013-11-01

Redox responsive nanotubes were fabricated by the template assisted layer-by-layer (LbL) assembly method and employed as platforms for molecular payload release. Positively and negatively charged organometallic poly(ferrocenylsilane)s (PFS) were used to construct the nanotubes, in combination with other polyions. During fabrication, multilayers of these polyions were deposited onto the inner pores of template porous membranes, followed by subsequent removal of the template. Anodized porous alumina and track-etched polycarbonate membranes were used as templates. The morphology, electrochemistry, composition and other properties of the obtained tubular structure were characterized by fluorescence microscopy, scanning (SEM) and transmission electron microscopy (TEM) and energy-dispersive X-ray (EDX) spectroscopy. Composite nanotubes, consisting of poly(acrylic acid) anions with PFS+ and nanoparticles including fluorophore labelled dextran and decorated quantum dots, with PFS polyelectrolytes were also fabricated, broadening the scope of the structures. Cyclic voltammograms of PFS containing nanotubes showed similar redox responsive behaviour to thin LbL assembled films. Redox triggered release of labelled macromolecules from these tubular structures demonstrated application potential in controlled molecular delivery.Redox responsive nanotubes were fabricated by the template assisted layer-by-layer (LbL) assembly method and employed as platforms for molecular payload release. Positively and negatively charged organometallic poly(ferrocenylsilane)s (PFS) were used to construct the nanotubes, in combination with other polyions. During fabrication, multilayers of these polyions were deposited onto the inner pores of template porous membranes, followed by subsequent removal of the template. Anodized porous alumina and track-etched polycarbonate membranes were used as templates. The morphology, electrochemistry, composition and other properties of the obtained tubular structure were characterized by fluorescence microscopy, scanning (SEM) and transmission electron microscopy (TEM) and energy-dispersive X-ray (EDX) spectroscopy. Composite nanotubes, consisting of poly(acrylic acid) anions with PFS+ and nanoparticles including fluorophore labelled dextran and decorated quantum dots, with PFS polyelectrolytes were also fabricated, broadening the scope of the structures. Cyclic voltammograms of PFS containing nanotubes showed similar redox responsive behaviour to thin LbL assembled films. Redox triggered release of labelled macromolecules from these tubular structures demonstrated application potential in controlled molecular delivery. Electronic supplementary information (ESI) available: Nanotube wall thickness determination protocol. See DOI: 10.1039/c3nr03927g

Bond strength of different adhesives to normal and caries-affected dentins.

PubMed

Xuan, Wei; Hou, Ben-xiang; Lü, Ya-lin

2010-02-05

Currently, several systems of dentin substrate-reacting adhesives are available for use in the restorative treatment against caries. However, the bond effectiveness and property of different adhesive systems to caries-affected dentin are not fully understood. The objective of this study was to evaluate the bond strength of different adhesives to both normal dentin (ND) and caries-affected dentin (CAD) and to analyze the dentin/adhesive interfacial characteristics. Twenty eight extracted human molars with coronal medium carious lesions were randomly assigned to four groups according to adhesives used. ND and CAD were bonded with etch-and-rinse adhesive Adper Single Bond 2 (SB2) or self-etching adhesives Clearfil SE Bond (CSE), Clearfil S(3) Bond (CS3), iBond GI (IB). Rectangular sticks of resin-dentin bonded interfaces 0.9 mm(2) were obtained. The specimens were subjected to microtensile bond strength (microTBS) testing at a crosshead speed of 1 mm/min. Mean microTBS was statistically analyzed with analysis of variance (ANOVA) and Student-Newman-Keuls tests. Interfacial morphologies were analyzed by Scanning Electron Microscopy (SEM). Etch-and-rinse adhesive Adper(TM) Single Bond 2 yielded high bond strength when applied to both normal and caries-affected dentin. The two-step self-etching adhesive Clearfil SE Bond generated the highest bond strength to ND among all adhesives tested but a significantly reduced strength when applied to CAD. For the one-step self-etching adhesives, Clearfil S(3) Bond and iBond GI, the bond strength was relatively low regardless of the dentin type. SEM interfacial analysis revealed that hybrid layers were thicker with poorer resin tag formation and less resin-filled lateral branches in the CAD than in the ND for all the adhesives tested. The etch-and-rinse adhesive performed more effectively to caries-affected dentin than the self-etching adhesives.

The impact of hydrofluoric acid etching followed by unfilled resin on the biaxial strength of a glass-ceramic.

PubMed

Posritong, Sumana; Borges, Alexandre Luiz Souto; Chu, Tien-Min Gabriel; Eckert, George J; Bottino, Marco A; Bottino, Marco C

2013-11-01

To evaluate the null hypotheses that hydrofluoric (HF) acid etching time would neither decrease the biaxial flexural strength of a glass-based veneering ceramic nor enhance it after silane and unfilled resin (UR) applications. Disc-shaped IPS e.max ZirPress specimens were allocated into 12 groups: G1-control (no-etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6-60 s+60 s. Groups (G7-G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology and roughness (Ra and Rq) of the ceramics were assessed by means of scanning electron microscopy (SEM) and profilometry, respectively. Flexural strength was determined by biaxial testing. Data were analyzed by two-way ANOVA and the Sidak test (α=0.05). Weibull statistics were estimated and finite element analysis (FEA) was carried out to verify the stress concentration end areas of fracture. The interaction (etching time vs. surface treatment) was significant for Ra (p=0.008) and Rq (0.0075). Resin-treated groups presented significantly lower Ra and Rq than non-treated groups, except for the 60s group (p<0.005). SEM revealed that etching affected the ceramic microstructure and that the UR was able to penetrate into the irregularities. A significant effect of etching time (p=0.029) on flexural strength was seen. G7-G12 presented higher strength than G1-G6 (p<0.0001). None of experimental groups failed to show 95% confidence intervals of σ0 and m overlapped. FEA showed lower stress concentration after resin treatment. HF acid etching time did not show a damaging effect on the ceramic flexural strength. Moreover, the flexural strength could be enhanced after UR treatment. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Biomechanical properties of jaw periosteum-derived mineralized culture on different titanium topography.

PubMed

Att, Wael; Kubo, Katsutoshi; Yamada, Masahiro; Maeda, Hatsuhiko; Ogawa, Takahiro

2009-01-01

This study evaluated the biomechanical properties of periosteum-derived mineralized culture on different surface topographies of titanium. Titanium surfaces modified by machining or by acid etching were analyzed using scanning electron microscopy (SEM). Rat mandibular periosteum-derived cells were cultured on either of the titanium surfaces. Cell proliferation was evaluated by cell counts, and gene expression was analyzed using a reverse-transcriptase polymerase chain reaction. Alkaline phosphatase (ALP) stain assay was employed to evaluate osteoblastic activity. Matrix mineralization was examined via von Kossa stain assay, total calcium deposition, and SEM. The hardness and elastic modulus of mineralized cultures were measured using a nano-indenter. The machined surface demonstrated a flat topographic configuration, while the acid-etched surface revealed a uniform micron-scale roughness. Both cell density and ALP activity were significantly higher on the machined surface than on the acid-etched surface. The expression of bone-related genes was up-regulated or enhanced on the acid-etched surface compared to the machined surface. Von Kossa stain showed significantly greater positive areas for the machined surface compared to the acid-etched surface, while total calcium deposition was statistically similar. Mineralized culture on the acid-etched surface was characterized by denser calcium deposition, more mature collagen deposition on the superficial layer, and larger and denser globular matrices inside the matrix than the culture on the machined surface. The mineralized matrix on the acid-etched surface was two times harder than on the machined surface, whereas the elastic modulus was comparable between the two surfaces. The design of this study can be used as a model to evaluate the effect of implant surface topography on the biomechanical properties of periosteum-derived mineralized culture. The results suggest that mandibular periosteal cells respond to different titanium surface topographies differently enough to produce mineralized matrices with different biomechanical qualities.

Effect of Storage Time on Bond Strength and Nanoleakage Expression of Universal Adhesives Bonded to Dentin and Etched Enamel.

PubMed

Makishi, P; André, C B; Ayres, Apa; Martins, A L; Giannini, M

2016-01-01

To investigate bond strength and nanoleakage expression of universal adhesives (UA) bonded to dentin and etched enamel. Extracted human third molars were sectioned and ground to obtain flat surfaces of dentin (n = 36) and enamel (n = 48). Dentin and etched enamel surfaces were bonded with one of two UAs, All-Bond Universal (ABU) or Scotchbond Universal (SBU); or a two-step self-etching adhesive, Clearfil SE Bond (CSEB). A hydrophobic bonding resin, Adper Scotchbond Multi-Purpose Bond (ASMP Bond) was applied only on etched enamel. Following each bonding procedure, resin composite blocks were built up incrementally. The specimens were sectioned and subjected to microtensile bond strength (MTBS) testing after 24 hours or one year water storage, or immersed into ammoniacal silver nitrate solution after aging with 10,000 thermocycles and observed using scanning electron microscopy. The percentage distribution of silver particles at the adhesive/tooth interface was calculated using digital image-analysis software. The MTBS (CSEB = SBU > ABU, for dentin; and CSEB > ABU = SBU = ASMP Bond, for etched enamel) differed significantly between the adhesives after 24 hours. After one year, MTBS values were reduced significantly within the same adhesive for both substrates (analysis of variance, Bonferroni post hoc, p<0.05), and no significant differences were found among the adhesives for etched enamel. Silver particles could be detected within the adhesive/dentin interface of all specimens tested. Kruskal-Wallis mean ranks for nanoleakage in ABU, SBU, and CSEB were 16.9, 18.5 and 11, respectively (p>0.05). In the short term, MTBS values were material and dental-substrate dependent. After aging, a decrease in bonding effectiveness was observed in all materials, with nanoleakage at the adhesive/dentin interface. The bonding of the UAs was equal or inferior to that of the conventional restorative systems when applied to either substrate and after either storage period.

Smoothing single-crystalline SiC surfaces by reactive ion etching using pure NF{sub 3} and NF{sub 3}/Ar mixture gas plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tasaka, Akimasa, E-mail: aki-tasaka-load@yahoo.co.jp; Kotaka, Yuki; Oda, Atsushi

2014-09-01

In pure NF{sub 3} plasma, the etching rates of four kinds of single-crystalline SiC wafer etched at NF{sub 3} pressure of 2 Pa were the highest and it decreased with an increase in NF{sub 3} pressure. On the other hand, they increased with an increase in radio frequency (RF) power and were the highest at RF power of 200 W. A smooth surface was obtained on the single-crystalline 4H-SiC after reactive ion etching at NF{sub 3}/Ar gas pressure of 2 Pa and addition of Ar to NF{sub 3} plasma increased the smoothness of SiC surface. Scanning electron microscopy observation revealed that the numbermore » of pillars decreased with an increase in the Ar-concentration in the NF{sub 3}/Ar mixture gas. The roughness factor (R{sub a}) values were decreased from 51.5 nm to 25.5 nm for the As-cut SiC, from 0.25 nm to 0.20 nm for the Epi-SiC, from 5.0 nm to 0.7 nm for the Si-face mirror-polished SiC, and from 0.20 nm to 0.16 nm for the C-face mirror-polished SiC by adding 60% Ar to the NF{sub 3} gas. Both the R{sub a} values of the Epi- and the C-face mirror-polished wafer surfaces etched using the NF{sub 3}/Ar (40:60) plasma were similar to that treated with mirror polishing, so-called the Catalyst-Referred Etching (CARE) method, with which the lowest roughness of surface was obtained among the chemical mirror polishing methods. Etching duration for smoothing the single-crystalline SiC surface using its treatment was one third of that with the CARE method.« less

Direct mapping and characterization of dry etch damage-induced PN junction for long-wavelength HgCdTe infrared detector arrays.

PubMed

Li, Yantao; Hu, Weida; Ye, Zhenhua; Chen, Yiyu; Chen, Xiaoshuang; Lu, Wei

2017-04-01

Mercury cadmium telluride is the standard material to fabricate high-performance infrared focal plane array (FPA) detectors. However, etch-induced damage is a serious obstacle for realizing highly uniform and damage-free FPA detectors. In this Letter, the high signal-to-noise ratio and high spatial resolution scanning photocurrent microscopy (SPCM) is used to characterize the dry etch-induced inversion layer of vacancy-doped p-type Hg_1-xCd_xTe (x=0.22) material under different etching temperatures. It is found that the peak-to-peak magnitude of the SPCM profile decreases with a decrease in etching temperature, showing direct proof of controlling dry etch-induced type conversion. Our work paves the way toward seeking optimal etching processes in large-scale infrared FPAs.

Electroless-plated Ni pattern with catalyst printing on indium-gallium-zinc oxide surface

NASA Astrophysics Data System (ADS)

Onoue, Miki; Ogura, Shintaro; Kusaka, Yasuyuki; Fukuda, Nobuko; Yamamoto, Noritaka; Kojima, Keisuke; Chikama, Katsumi; Ushijima, Hirobumi

2017-05-01

Electroless plated metals have been used for wiring and electrodes in the manufacture of electronic devices. To obtain plated patterns, etching and photoresist are generally used. However, through catalyst patterning by printing, we can obtain metal patterns without etching and photoresists by electroless plating. Solution-processed indium-gallium-zinc oxide (IGZO) has received significant attention for showing high performance and ease of preparation in air atmosphere. In this study, we prepared an electroless plated pattern by catalyst printing as electrodes of IGZO TFT. There are few reports on the application of plated metal electrodes prepared by catalyst printing to the source and drain electrodes of IGZO TFT. The prepared IGZO TFT exhibits a typical current-voltage (I-V) curve. The plated electrodes caused many problems such as performance degradation. However, our result showed that the plated metal electrodes can drive IGZO TFT. In addition, we confirm plated metal growth into the catalyst layer by cross sectional scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM/EDS) of the plated Ni. We discuss the relevance of the measured work function (WF) of the electrode materials and the performance of IGZO TFT.

Environmental scanning electron microscope imaging examples related to particle analysis.

PubMed

Wight, S A; Zeissler, C J

1993-08-01

This work provides examples of some of the imaging capabilities of environmental scanning electron microscopy applied to easily charged samples relevant to particle analysis. Environmental SEM (also referred to as high pressure or low vacuum SEM) can address uncoated samples that are known to be difficult to image. Most of these specimens are difficult to image by conventional SEM even when coated with a conductive layer. Another area where environmental SEM is particularly applicable is for specimens not compatible with high vacuum, such as volatile specimens. Samples from which images were obtained that otherwise may not have been possible by conventional methods included fly ash particles on an oiled plastic membrane impactor substrate, a one micrometer diameter fiber mounted on the end of a wire, uranium oxide particles embedded in oil-bearing cellulose nitrate, teflon and polycarbonate filter materials with collected air particulate matter, polystyrene latex spheres on cellulosic filter paper, polystyrene latex spheres "loosely" sitting on a glass slide, and subsurface tracks in an etched nuclear track-etch detector. Surface charging problems experienced in high vacuum SEMs are virtually eliminated in the low vacuum SEM, extending imaging capabilities to samples previously difficult to use or incompatible with conventional methods.

Cryogenic Etching of Silicon: An Alternative Method For Fabrication of Vertical Microcantilever Master Molds

PubMed Central

Addae-Mensah, Kweku A.; Retterer, Scott; Opalenik, Susan R.; Thomas, Darrell; Lavrik, Nickolay V.; Wikswo, John P.

2013-01-01

This paper examines the use of deep reactive ion etching (DRIE) of silicon with fluorine high-density plasmas at cryogenic temperatures to produce silicon master molds for vertical microcantilever arrays used for controlling substrate stiffness for culturing living cells. The resultant profiles achieved depend on the rate of deposition and etching of a SiOxFy polymer, which serves as a passivation layer on the sidewalls of the etched structures in relation to areas that have not been passivated with the polymer. We look at how optimal tuning of two parameters, the O2 flow rate and the capacitively coupled plasma (CCP) power, determine the etch profile. All other pertinent parameters are kept constant. We examine the etch profiles produced using e-beam resist as the main etch mask, with holes having diameters of 750 nm, 1 µm, and 2 µm. PMID:24223478

DOE Office of Scientific and Technical Information (OSTI.GOV)

Belomoin, Gennadiy; Therrien, Joel; Nayfeh, Munir

We dispersed electrochemical etched silicon into a colloid of ultrasmall ultrabright Si nanoparticles. Direct imaging using transmission electron microscopy shows particles of {approx}1 nm in diameter, and infrared and electron photospectroscopy show that they are passivated with hydrogen. Under 350 nm excitation, the luminescence is dominated by an extremely strong blue band at 390 nm. We replace hydrogen by a high-quality ultrathin surface oxide cap by self-limiting oxidation in H{sub 2}O{sub 2}. Upon capping, the excitation efficiency drops, but only by a factor of 2, to an efficiency still two-fold larger than that of fluorescein. Although of slightly lower brightness,more » capped Si particles have superior biocompatability, an important property for biosensing applications. (c) 2000 American Institute of Physics.« less

Synthesis of high aspect ratio ZnO nanowires with an inexpensive handcrafted electrochemical setup

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taheri, Ali, E-mail: at1361@aut.ac.ir, E-mail: atahery@aeoi.org.ir; Saramad, Shahyar; Setayeshi, Saeed

In this work, high aspect ratio zinc oxide nanowires are synthesized using templated one-step electrodeposition technique. Electrodeposition of the nanowires is done using a handcrafted electronic system. Nuclear track-etched polycarbonate membrane is used as a template to form the high aspect ratio nanowires. The result of X-ray diffraction and scanning electron microscopy shows that nanowires with a good crystallinity and an aspect ratio of more than 30 can be achieved in a suitable condition. The height of electrodeposited nanowires reaches to about 11 μm. Based on the obtained results, high aspect ratio ZnO nanowires can be formed using inexpensive electrodepositionmore » setup with an acceptable quality.« less

Smooth and vertical facet formation for AlGaN-based deep-UV laser diodes.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bogart, Katherine Huderle Andersen; Shul, Randy John; Stevens, Jeffrey

2008-10-01

Using a two-step method of plasma and wet chemical etching, we demonstrate smooth, vertical facets for use in Al{sub x} Ga{sub 1-x} N-based deep-ultraviolet laser-diode heterostructures where x = 0 to 0.5. Optimization of plasma-etching conditions included increasing both temperature and radiofrequency (RF) power to achieve a facet angle of 5 deg from vertical. Subsequent etching in AZ400K developer was investigated to reduce the facet surface roughness and improve facet verticality. The resulting combined processes produced improved facet sidewalls with an average angle of 0.7 deg from vertical and less than 2-nm root-mean-square (RMS) roughness, yielding an estimated reflectivity greatermore » than 95% of that of a perfectly smooth and vertical facet.« less

Cardiac Mitochondria l Membrane Stability after Deep Hypothermia using a Xenon Clathrate Cryostasis Protocol – an Electron Microscopy Study

PubMed Central

Sheleg, Sergey; Hixon, Hugh; Cohen, Bruce; Lowry, David; Nedzved, Mikhail

2008-01-01

We investigated a new cryopreservation method using xenon, a clathrate-forming gas, under medium pressure (100psi). The objective of the study was to determine whether this cryostasis protocol could protect cardiac mitochondria at cryogenic temperatures (below 100 degrees Celsius).We analyzed transmission electron microscopy images to obtain information about changes in mitochondrial morphology induced by cryopreservation of the hearts. Our data showed absence of mitochondrial swelling, rupture of inner and outer membranes, and leakage of mitochondrial matrix into the cytoplasm after applying this cryostasis protocol. The electron microscopy results provided the first evidence that a cryostasis protocol using xenon as a clathrate-forming gas under pressure may have protective effects on intracellular membranes. This cryostasis technology may find applications in developing new approaches for long-term cryopreservation protocols. PMID:18787624

Bulk vertical micromachining of single-crystal sapphire using inductively coupled plasma etching for x-ray resonant cavities

NASA Astrophysics Data System (ADS)

Chen, P.-C.; Lin, P.-T.; Mikolas, D. G.; Tsai, Y.-W.; Wang, Y.-L.; Fu, C.-C.; Chang, S.-L.

2015-01-01

To provide coherent x-ray sources for probing the dynamic structures of solid or liquid biological substances on the picosecond timescale, a high-aspect-ratio x-ray resonator cavity etched from a single crystal substrate with a nearly vertical sidewall structure is required. Although high-aspect-ratio resonator cavities have been produced in silicon, they suffer from unwanted multiple beam effects. However, this problem can be avoided by using the reduced symmetry of single-crystal sapphire in which x-ray cavities may produce a highly monochromatic transmitted x-ray beam. In this study, we performed nominal 100 µm deep etching and vertical sidewall profiles in single crystal sapphire using inductively coupled plasma (ICP) etching. The large depth is required to intercept a useful fraction of a stopped-down x-ray beam, as well as for beam clearance. An electroplated Ni hard mask was patterned using KMPR 1050 photoresist and contact lithography. The quality and performance of the x-ray cavity depended upon the uniformity of the cavity gap and therefore verticality of the fabricated vertical sidewall. To our knowledge, this is the first report of such deep, vertical etching of single-crystal sapphire. A gas mixture of Cl2/BCl3/Ar was used to etch the sapphire with process variables including BCl3 flow ratio and bias power. By etching for 540 min under optimal conditions, we obtained an x-ray resonant cavity with a depth of 95 µm, width of ~30 µm, gap of ~115 µm and sidewall profile internal angle of 89.5°. The results show that the etching parameters affected the quality of the vertical sidewall, which is essential for good x-ray resonant cavities.

Fabrication of ultra-high aspect ratio (>160:1) silicon nanostructures by using Au metal assisted chemical etching

NASA Astrophysics Data System (ADS)

Li, Hailiang; Ye, Tianchun; Shi, Lina; Xie, Changqing

2017-12-01

We present a facile and effective approach for fabricating high aspect ratio, dense and vertical silicon nanopillar arrays, using a combination of metal etching following electron-beam lithography and Au metal assisted chemical etching (MacEtch). Ti/Au nanostructures used as catalysts in MacEtch are formed by single layer resist-based electron-beam exposure followed by ion beam etching. The effects of MacEtch process parameters, including half period, etching time, the concentrations of H2O2 and HF, etching temperature and drying method are systematically investigated. Especially, we demonstrate an enhancement of etching quality by employing cold MacEtch process, and an enhancement in preventing the collapse of high aspect ratio nanostructures by employing low surface tension rinse liquid and natural evaporation in the drying stage. Using an optimized MacEtch process, vertical silicon nanopillar arrays with a period of 250 nm and aspect ratio up to 160:1 are realized. Our results should be instructive for exploring the achievable aspect ratio limit in silicon nanostructures and may find potential applications in photovoltaic devices, thermoelectric devices and x-ray diffractive optics.

Hierarchical micro-nano structured Ti6Al4V surface topography via two-step etching process for enhanced hydrophilicity and osteoblastic responses.

PubMed

Moon, Byeong-Seok; Kim, Sungwon; Kim, Hyoun-Ee; Jang, Tae-Sik

2017-04-01

Hierarchical micro-nano (HMN) surface structuring of dental implants is a fascinating strategy for achieving fast and mechanically stable fixation due to the synergetic effect of micro- and nano-scale surface roughness with surrounding tissues. However, the introduction of a well-defined nanostructure on a microstructure having complex surface geometry is still challenging. As a means of fabricating HMN surface on Ti6Al4V-ELI, target-ion induced plasma sputtering (TIPS) was used onto a sand-blasted, large-grit and acid-etched substrate. The HMN surface topography was simply controlled by adjusting the tantalum (Ta) target power of the TIPS technique, which is directly related to the Ta ion flux and the surface chemical composition of the substrate. Characterization using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and laser scanning microscopy (LSM) verified that well-defined nano-patterned surface structures with a depth of ~300 to 400nm and a width of ~60 to 70nm were uniformly distributed and followed the complex micron-sized surface geometry. In vitro cellular responses of pre-osteoblast cells (MC3T3-E1) were assessed by attachment and proliferation of cells on flat, nano-roughened, micro-roughened, and an HMN surface structure of Ti6Al4V-ELI. Moreover, an in vivo dog mandible defect model study was used to investigate the biological effect of the HMN surface structure compared with the micro-roughened surface. The results showed that the surface nanostructure significantly increased the cellular activities of flat and micro-roughened Ti, and the bone-to-implant contact area and new bone volume were significantly improved on the HMN surface structured Ti. These results support the idea that an HMN surface structure on Ti6Al4V-ELI alloy has great potential for enhancing the biological performance of dental implants. Copyright © 2016 Elsevier B.V. All rights reserved.

Identification of sigma and chi phases in duplex stainless steels

DOE Office of Scientific and Technical Information (OSTI.GOV)

Llorca-Isern, Núria, E-mail: nullorca@ub.edu; López-Luque, Héctor, E-mail: hlopezlu7@alumnes.ub.edu; López-Jiménez, Isabel, E-mail: ilopezji9@alumnes.ub.edu

The aim of this work is to find out the most suitable method for detecting and analyzing accurately the formation conditions of secondary phases, particularly Sigma-phase (σ-phase) and Chi-phase (χ-phase) in duplex stainless steels (UNS S32205 and UNS S32750). The microstructure was characterized after a solution annealing at 1080 °C followed by an isothermal heating at 830 °C for different time ranges, ranging from 1 min to 9 h, in order to enlighten the controversial point concerning the mechanism of χ-phase nucleation in relation with the σ-phase. Etched samples were observed using optical microscopy (MO), and scanning electron microscopy (FESEM)more » with a backscattered electron detector (BSE) was used on unetched samples. Compositional microanalysis (EDS) was carried out for identifying the different phases present in the steels. Sigma phase was easily observed using different etching procedures, whereas χ-phase was only clearly detected with FESEM–BSE on unetched samples. The compositional analyses showed that the molybdenum content in χ-phase almost doubles the content of this element in σ-phase, and as a result the kinetics of nucleation and growth were also found to be remarkably faster when the alloy content in the steel is higher. In addition, chromium nitrides and carbides were also observed to precipitate as a result of the heat treatments and, in the case of the chromium nitrides, they act as a favorable site for the nucleation of σ-phase and χ-phase. - Highlights: • Microscopy was used on heat treated duplex steels for microstructure identification. • FESEM–BSE observation on unetched samples provided the best contrast between phases. • Analyses of carbides, nitrides, chi and sigma phases were possible by EDS and WDS. • Chromium nitrides act as favorable site for the nucleation of chi and sigma phases. • Secondary phases nucleation kinetics are faster in superduplex than in duplex steels.« less

Thermal ink-jet device using single-chip silicon microchannels

NASA Astrophysics Data System (ADS)

Wuu, DongSing; Cheng, Chen-Yue; Horng, RayHua; Chan, G. C.; Chiu, Sao-Ling; Wu, Yi-Yung

1998-06-01

We present a new method to fabricate silicon microfluidic channels by through-hole etching with subsequent planarization. The method is based on etching out the deep grooves through a perforated silicon carbide membrane, followed by sealing the membrane with plasma-enhanced chemical vapor deposition (PECVD). Low-pressure-chemical-vapor- deposited (LPCVD) polysilicon was used as a sacrificial layer to define the channel structure and only one etching step is required. This permits the realization of planarization after a very deep etching step in silicon and offers the possibility for film deposition, resist spinning and film patterning across deep grooves. The process technology was demonstrated on the fabrication of a monolithic silicon microchannel structure for thermal inkjet printing. The Ta-Al heater arrays are integrated on the top of each microchannel, which connect to a common on-chip front-end ink reservoir. The fabrication of this device requires six masks and no active nozzle-to-chip alignment. Moreover, the present micromachining process is compatible with the addition of on-chip circuitry for multiplexing the heater control signals. Heat transfer efficiency to the ink is enhanced by the high thermal conductivity of the silicon carbide in the channel ceiling, while the bulk silicon maintains high interchannel isolation. The fabricated inkjet devices show the droplet sizes of 20 - 50 micrometer in diameter with various channel dimensions and stable ejection of ink droplets more than 1 million.

Comparison of fabrication methods for microstructured deep UV multimode waveguides based on fused silica

NASA Astrophysics Data System (ADS)

Elmlinger, Philipp; Schreivogel, Martin; Schmid, Marc; Kaiser, Myriam; Priester, Roman; Sonström, Patrick; Kneissl, Michael

2016-04-01

The suitability of materials for deep ultraviolet (DUV) waveguides concerning transmittance, fabrication, and coupling properties is investigated and a fused silica core/ambient air cladding waveguide system is presented. This high refractive index contrast system has far better coupling efficiency especially for divergent light sources like LEDs and also a significantly smaller critical bending radius compared to conventional waveguide systems, as simulated by ray-tracing simulations. For the fabrication of 300-ffm-thick multimode waveguides a hydrouoric (HF) acid based wet etch process is compared to selective laser etching (SLE). In order to fabricate thick waveguides out of 300-ffm-thick silica wafers by HF etching, two masking materials, LPCVD silicon nitride and LPCVD poly silicon, are investigated. Due to thermal stress, the silicon nitride deposited wafers show cracks and even break. Using poly silicon as a masking material, no cracks are observed and deep etching in 50 wt% HF acid up to 180 min is performed. While the masked and unmasked silica surface is almost unchanged in terms of roughness, notching defects occur at the remaining polysilicon edge leading to jagged sidewalls. Using SLE, waveguides with high contour accuracy are fabricated and the DUV guiding properties are successfully demonstrated with propagation losses between 0.6 and 0:8 dB=mm. These values are currently limited by sidewall scattering losses.

Method for providing an arbitrary three-dimensional microstructure in silicon using an anisotropic deep etch

DOEpatents

Morales, Alfredo M.; Gonzales, Marcela

2004-06-15

The present invention describes a method for fabricating an embossing tool or an x-ray mask tool, providing microstructures that smoothly vary in height from point-to-point in etched substrates, i.e., structure which can vary in all three dimensions. The process uses a lithographic technique to transfer an image pattern in the surface of a silicon wafer by exposing and developing the resist and then etching the silicon substrate. Importantly, the photoresist is variably exposed so that when developed some of the resist layer remains. The remaining undeveloped resist acts as an etchant barrier to the reactive plasma used to etch the silicon substrate and therefore provides the ability etch structures of variable depths.

A Widely-Accessible Distributed MEMS Processing Environment. The MEMS Exchange Program

DTIC Science & Technology

2012-10-29

promise for high-aspect and deep etching into fused silica. This process capability is important for a DARPA project called the Navigation-Grade...on fused silica samples that appear to allow 2 to 1 aspect ratios in fused silica with a depth of etch of around 125 microns – a dramatic result in a...very hard to etch material such as fused silica! After receiving approval from DARPA, the MEMS Exchange purchased a previously- owned Ulvac etcher

Multi-Step Deep Reactive Ion Etching Fabrication Process for Silicon-Based Terahertz Components

NASA Technical Reports Server (NTRS)

Reck, Theodore (Inventor); Perez, Jose Vicente Siles (Inventor); Lee, Choonsup (Inventor); Cooper, Ken B. (Inventor); Jung-Kubiak, Cecile (Inventor); Mehdi, Imran (Inventor); Chattopadhyay, Goutam (Inventor); Lin, Robert H. (Inventor); Peralta, Alejandro (Inventor)

2016-01-01

A multi-step silicon etching process has been developed to fabricate silicon-based terahertz (THz) waveguide components. This technique provides precise dimensional control across multiple etch depths with batch processing capabilities. Nonlinear and passive components such as mixers and multipliers waveguides, hybrids, OMTs and twists have been fabricated and integrated into a small silicon package. This fabrication technique enables a wafer-stacking architecture to provide ultra-compact multi-pixel receiver front-ends in the THz range.

Formation and metrology of dual scale nano-morphology on SF(6) plasma etched silicon surfaces.

PubMed

Boulousis, G; Constantoudis, V; Kokkoris, G; Gogolides, E

2008-06-25

Surface roughness and nano-morphology in SF(6) plasma etched silicon substrates are investigated in a helicon type plasma reactor as a function of etching time and process parameters. The plasma etched surfaces are analyzed by atomic force microscopy. It is found that dual scale nano-roughness is formatted on the silicon surface comprising an underlying nano-roughness and superimposed nano-mounds. Detailed metrological quantification is proposed for the characterization of dual scale surface morphology. As etching proceeds, the mounds become higher, fewer and wider, and the underlying nano-roughness also increases. Increase in wafer temperature leads to smoother surfaces with lower, fewer and wider nano-mounds. A mechanism based on the deposition of etch inhibiting particles during the etching process is proposed for the explanation of the experimental behavior. In addition, appropriately designed experiments are conducted, and they confirm the presence of this mechanism.

A deep convolutional neural network approach to single-particle recognition in cryo-electron microscopy.

PubMed

Zhu, Yanan; Ouyang, Qi; Mao, Youdong

2017-07-21

Single-particle cryo-electron microscopy (cryo-EM) has become a mainstream tool for the structural determination of biological macromolecular complexes. However, high-resolution cryo-EM reconstruction often requires hundreds of thousands of single-particle images. Particle extraction from experimental micrographs thus can be laborious and presents a major practical bottleneck in cryo-EM structural determination. Existing computational methods for particle picking often use low-resolution templates for particle matching, making them susceptible to reference-dependent bias. It is critical to develop a highly efficient template-free method for the automatic recognition of particle images from cryo-EM micrographs. We developed a deep learning-based algorithmic framework, DeepEM, for single-particle recognition from noisy cryo-EM micrographs, enabling automated particle picking, selection and verification in an integrated fashion. The kernel of DeepEM is built upon a convolutional neural network (CNN) composed of eight layers, which can be recursively trained to be highly "knowledgeable". Our approach exhibits an improved performance and accuracy when tested on the standard KLH dataset. Application of DeepEM to several challenging experimental cryo-EM datasets demonstrated its ability to avoid the selection of un-wanted particles and non-particles even when true particles contain fewer features. The DeepEM methodology, derived from a deep CNN, allows automated particle extraction from raw cryo-EM micrographs in the absence of a template. It demonstrates an improved performance, objectivity and accuracy. Application of this novel method is expected to free the labor involved in single-particle verification, significantly improving the efficiency of cryo-EM data processing.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vazehrad, S., E-mail: vazehrad@kth.se; Elfsberg, J., E-mail: jessica.elfsberg@scania.com; Diószegi, A., E-mail: attila.dioszegi@jth.hj.se

An investigation on silicon segregation of lamellar, compacted and nodular graphite iron was carried out by applying a selective, immersion color etching and a modified electron microprobe to study the microstructure. The color etched micrographs of the investigated cast irons by revealing the austenite phase have provided data about the chronology and mechanism of microstructure formation. Moreover, electron microprobe has provided two dimensional segregation maps of silicon. A good agreement was found between the segregation profile of silicon in the color etched microstructure and the silicon maps achieved by electron microprobe analysis. However, quantitative silicon investigation was found to bemore » more accurate than color etching results to study the size of the eutectic colonies. - Highlights: • Sensitivity of a color etchant to silicon segregation is quantitatively demonstrated. • Si segregation measurement by EMPA approved the results achieved by color etching. • Color etched micrographs provided data about solidification mechanism in cast irons. • Austenite grain boundaries were identified by measuring the local Si concentration.« less

Size exclusion chromatography for semipreparative scale separation of Au38(SR)24 and Au40(SR)24 and larger clusters.

PubMed

Knoppe, Stefan; Boudon, Julien; Dolamic, Igor; Dass, Amala; Bürgi, Thomas

2011-07-01

Size exclusion chromatography (SEC) on a semipreparative scale (10 mg and more) was used to size-select ultrasmall gold nanoclusters (<2 nm) from polydisperse mixtures. In particular, the ubiquitous byproducts of the etching process toward Au(38)(SR)(24) (SR, thiolate) clusters were separated and gained in high monodispersity (based on mass spectrometry). The isolated fractions were characterized by UV-vis spectroscopy, MALDI mass spectrometry, HPLC, and electron microscopy. Most notably, the separation of Au(38)(SR)(24) and Au(40)(SR)(24) clusters is demonstrated.

Do matrix metalloproteinase inhibitors improve the bond durability of universal dental adhesives?

PubMed

Tekçe, Neslihan; Tuncer, Safa; Demirci, Mustafa; Balci, Sibel

2016-11-01

The aim of this study was to evaluate the effects of matrix metalloproteinases (MMPs) inhibitors on the microtensile bond strength (μTBS) and the adhesive-dentin interface of two universal dentin bonding agents, Single Bond Universal and All Bond Universal, after 12 months of water storage. Seventy extracted, caries-free, human third molars were used in this study. Of these, 50 were used for μTBS testing and 20 were used for scanning electron microscopy. The two bonding agents were applied to flat dentin surfaces in five different ways: self-etch mode, etch-and-rinse mode with 37% phosphoric acid, etch-and-rinse mode with phosphoric acid containing 1% benzalkonium chloride, etch-and-rinse mode with phosphoric acid and 2% chlorhexidine, and etch-and-rinse mode with 0.5 M ethylenediaminetetraacetic acid (EDTA) (n = 5 for each bonding agent in each group; N = 50). Half the specimens were subjected to μTBS tests at 24 h, while half were subjected to the tests after 12 months of water storage. For each bonding agent, inhibition, storage, and their interaction effects were tested by two-way analysis of variance and Bonferroni tests. For Single Bond Universal, the benzalkonium chloride (p = 0.024) and chlorhexidine groups (p = 0.033) exhibited significantly higher μTBS values at 24 h compared with the self-etch group. For All Bond Universal, all groups displayed similar bond strengths at 24 h (p > 0.05). After 12 months of water storage, the μTBS values decreased significantly in the benzalkonium chloride group for Single Bond Universal (p = 0.001) and the self-etch (p = 0.029), chlorhexidine (p = 0.046), and EDTA (p = 0.032) groups for All Bond Universal. These results suggest that the immediate dentin bond strength increases when universal bonding systems are applied in the etch-and-rinse mode, although the durability decreases. The use of chlorhexidine and EDTA can increase the bond durability of mild adhesives such as Single Bond Universal. SCANNING 38:535-544, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Effect of acid etching on bond strength of nanoionomer as an orthodontic bonding adhesive

PubMed Central

Khan, Saba; Verma, Sanjeev K.; Maheshwari, Sandhya

2015-01-01

Aims: A new Resin Modified Glass Ionomer Cement known as nanoionomer containing nanofillers of fluoroaluminosilicate glass and nanofiller 'clusters' has been introduced. An in-vitro study aimed at evaluating shear bond strength (SBS) and adhesive remnant index (ARI) of nanoionomer under etching/unetched condition for use as an orthodontic bonding agent. Material and Methods: A total of 75 extracted premolars were used, which were divided into three equal groups of 25 each: 1-Conventional adhesive (Enlight Light Cure, SDS, Ormco, CA, USA) was used after and etching with 37% phosphoric acid for 30 s, followed by Ortho Solo application 2-nanoionomer (Ketac™ N100, 3M, ESPE, St. Paul, MN, USA) was used after etching with 37% phosphoric acid for 30 s 3-nanoionomer was used without etching. The SBS testing was performed using a digital universal testing machine (UTM-G-410B, Shanta Engineering). Evaluation of ARI was done using scanning electron microscopy. The SBS were compared using ANOVA with post-hoc Tukey test for intergroup comparisons and ARI scores were compared with Chi-square test. Results: ANOVA (SBS, F = 104.75) and Chi-square (ARI, Chi-square = 30.71) tests revealed significant differences between groups (P < 0.01). The mean (SD) SBS achieved with conventional light cure adhesive was significantly higher (P < 0.05) (10.59 ± 2.03 Mpa, 95% CI, 9.74-11.41) than the nanoionomer groups (unetched 4.13 ± 0.88 Mpa, 95% CI, 3.79-4.47 and etched 9.32 ± 1.87 Mpa, 95% CI, 8.58-10.06). However, nanoionomer with etching, registered SBS in the clinically acceptable range of 5.9–7.8 MPa, as suggested by Reynolds (1975). The nanoionomer groups gave significantly lower ARI values than the conventional adhesive group. Conclusion: Based on this in-vitro study, nanoionomer with etching can be successfully used as an orthodontic bonding agent leaving less adhesive remnant on enamel surface, making cleaning easier. However, in-vivo studies are needed to confirm the validity of present findings. PMID:26955629

Preparation of etched tantalum semimicro capacitor stimulation electrodes.

PubMed

Robblee, L S; Kelliher, E M; Langmuir, M E; Vartanian, H; McHardy, J

1983-03-01

The ideal electrode for stimulation of the nervous system is one that will inject charge by purely capacitive processes. One approach is to exploit the type of metal-oxide combination used in electrolytic capacitors, e.g., Ta/Ta2O5. For this purpose, fine tantalum wire (0.25 mm diam) was etched electrolytically at constant current in a methanol solution of NH4Br containing 1.5 wt % H2O. Electrolytic etching produced a conical tip with a length of ca. 0.5 mm and shaft diameters ranging from 0.10 to 0.16 mm. The etched electrodes were anodized to 10 V (vs. SCE) in 0.1 vol % H3PO4. The capacitance values normalized to geometric area of etched electrodes ranged from 0.13 to 0.33 micro F mm-2. Comparison of these values to the capacitance of "smooth" tantalum anodized to 10 V (0.011 micro F mm-2) indicated that the degree of surface enhancement, or etch ratio, was 12-30. The surface roughness was confirmed by scanning electron microscopy studies which revealed an intricate array of irregularly shaped surface projections about 1-2 micrometers wide. The etched electrodes were capable of delivering 0.06-0.1 micro C of charge with 0.1 ms pulses at a pulse repetition rate of 400 Hz when operated at 50% of the anodization voltage. This quantity of charge corresponded to volumetric charge densities of 20-30 micro C mm-3 and area charge densities of 0.55-0.88 micro C mm-2. Charge storage was proportionately higher at higher fractional values of the formation voltage. Leakage currents at 5 V were ca. 2 nA. Neither long-term passive storage (1500 h) nor extended pulsing time (18 h) had a deleterious effect on electrode performance. The trend in electrical stimulation work is toward smaller electrodes. The procedures developed in this study should be particularly well-suited to the fabrication of even smaller electrodes because of the favorable electrical and geometric characteristics of the etched surface.

Bond strength of a pit-and-fissure sealant associated to etch-and-rinse and self-etching adhesive systems to saliva-contaminated enamel: individual vs. simultaneous light curing.

PubMed

Gomes-Silva, Jaciara Miranda; Torres, Carolina Paes; Contente, Marta Maria Martins Giamatei; Oliveira, Maria Angélica Hueb de Menezes; Palma-Dibb, Regina Guenka; Borsatto, Maria Cristina

2008-01-01

This study evaluated in vitro the shear bond strength (SBS) of a resin-based pit-and-fissure sealant [Fluroshield (F), Dentsply/Caulk] associated with either an etch-and-rinse [Adper Single Bond 2 (SB), 3M/ESPE] or a self-etching adhesive system [Clearfil S3 Bond (S3), Kuraray Co., Ltd.] to saliva-contaminated enamel, comparing two curing protocols: individual light curing of the adhesive system and the sealant or simultaneous curing of both materials. Mesial and distal enamel surfaces from 45 sound third molars were randomly assigned to 6 groups (n=15), according to the bonding technique: I - F was applied to 37% phosphoric acid etched enamel. The other groups were contaminated with fresh human saliva (0.01 mL; 10 s) after acid etching: II - SB and F were light cured separately; III - SB and F were light cured together; IV - S3 and F were light cured separately; V - S3 and F were light cured simultaneously; VI - F was applied to saliva-contaminated, acid-etched enamel without an intermediate bonding agent layer. SBS was tested to failure in a universal testing machine at 0.5 mm/min. Data were analyzed by one-way ANOVA and Fisher's test (alpha=0.05).The debonded specimens were examined with a stereomicroscope to assess the failure modes. Three representative specimens from each group were observed under scanning electron microscopy for a qualitative analysis. Mean SBS in MPa were: I-12.28 (+/-4.29); II-8.57 (+/-3.19); III-7.97 (+/-2.16); IV-12.56 (+/-3.11); V-11.45 (+/-3.77); and VI-7.47 (+/-1.99). In conclusion, individual or simultaneous curing of the intermediate bonding agent layer and the resin sealant did not seem to affect bond strength to saliva-contaminated enamel. S3/F presented significantly higher SBS than the that of the groups treated with SB etch-and-rinse adhesive system and similar SBS to that of the control group, in which the sealant was applied under ideal dry, noncontaminated conditions.

Decalin-assisted light emitting porous Si formation and its optical, surface and morphological properties

NASA Astrophysics Data System (ADS)

Karatutlu, Ali; Istengir, Sumeyra; Cosgun, Sedat; Seker, Isa; Unal, Bayram

2017-11-01

In this research paper, light emitting porous silicon (Lep-Si) samples were fabricated by a surfactant-mediated chemical stain etching solution in order to form homogenous luminescent nanostructures at room temperature. As an industrially important solvent, decalin (decahydronaphtalene) was used as a surfactant in the HF/HNO3 solutions in order to control the etching process. Morphological, surface and optical properties of the Lep-Si samples were examined using atomic force microscopy, X-ray photoelectron spectroscopy, photoluminescence (PL) spectroscopy, and laser scanning confocal microscopy (LSCM) techniques. These characterization techniques were correlated with the various etching times including depth dependent luminescence profiles for the first time. We report the optimum conditions for production of the most efficient Lep-Si using decalin (decahydronaphtalene) and possible structural origins of light emission using the depth dependent luminescence measurements.

Inductively Coupled Plasma and Electron Cyclotron Resonance Plasma Etching of InGaAlP Compound Semiconductor System

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abernathy, C.R.; Hobson, W.S.; Hong, J.

1998-11-04

Current and future generations of sophisticated compound semiconductor devices require the ability for submicron scale patterning. The situation is being complicated since some of the new devices are based on a wider diversity of materials to be etched. Conventional IUE (Reactive Ion Etching) has been prevalent across the industry so far, but has limitations for materials with high bond strengths or multiple elements. IrI this paper, we suggest high density plasmas such as ECR (Electron Cyclotron Resonance) and ICP (Inductively Coupled Plasma), for the etching of ternary compound semiconductors (InGaP, AIInP, AlGaP) which are employed for electronic devices like heterojunctionmore » bipolar transistors (HBTs) or high electron mobility transistors (HEMTs), and photonic devices such as light-emitting diodes (LEDs) and lasers. High density plasma sources, opeiating at lower pressure, are expected to meet target goals determined in terms of etch rate, surface morphology, surface stoichiometry, selectivity, etc. The etching mechanisms, which are described in this paper, can also be applied to other III-V (GaAs-based, InP-based) as well as III-Nitride since the InGaAIP system shares many of the same properties.« less

Porous Si nanowires for highly selective room-temperature NO2 gas sensing

NASA Astrophysics Data System (ADS)

Kwon, Yong Jung; Mirzaei, Ali; Gil Na, Han; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Oum, Wansik; Kim, Sang Sub; Kim, Hyoun Woo

2018-07-01

We report the room-temperature sensing characteristics of Si nanowires (NWs) fabricated from p-Si wafers by a metal-assisted chemical etching method, which is a facile and low-cost method. X-ray diffraction was used to the the study crystallinity and phase formation of Si NWs, and product morphology was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After confirmation of Si NW formation via the SEM and TEM micrographs, sensing tests were carried out at room temperature, and it was found that the Si NW sensor prepared from Si wafers with a resistivity of 0.001–0.003 Ω.cm had the highest response to NO2 gas (Rg/Ra = 1.86 for 50 ppm NO2), with a fast response (15 s) and recovery (30 s) time. Furthermore, the sensor responses to SO2, toluene, benzene, H2, and ethanol were nearly negligible, demonstrating the excellent selectivity to NO2 gas. The gas-sensing mechanism is discussed in detail. The present sensor can operate at room temperature, and is compatible with the microelectronic fabrication process, demonstrating its promise for next-generation Si-based electronics fused with functional chemical sensors.

Porous Si nanowires for highly selective room-temperature NO2 gas sensing.

PubMed

Kwon, Yong Jung; Mirzaei, Ali; Na, Han Gil; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Oum, Wansik; Kim, Sang Sub; Kim, Hyoun Woo

2018-07-20

We report the room-temperature sensing characteristics of Si nanowires (NWs) fabricated from p-Si wafers by a metal-assisted chemical etching method, which is a facile and low-cost method. X-ray diffraction was used to the the study crystallinity and phase formation of Si NWs, and product morphology was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After confirmation of Si NW formation via the SEM and TEM micrographs, sensing tests were carried out at room temperature, and it was found that the Si NW sensor prepared from Si wafers with a resistivity of 0.001-0.003 Ω.cm had the highest response to NO 2 gas (R g /R a  = 1.86 for 50 ppm NO 2 ), with a fast response (15 s) and recovery (30 s) time. Furthermore, the sensor responses to SO 2 , toluene, benzene, H 2 , and ethanol were nearly negligible, demonstrating the excellent selectivity to NO 2 gas. The gas-sensing mechanism is discussed in detail. The present sensor can operate at room temperature, and is compatible with the microelectronic fabrication process, demonstrating its promise for next-generation Si-based electronics fused with functional chemical sensors.

Tailoring Co(OH)2 hollow nanostructures via Cu2O template etching for high performance supercapacitors.

PubMed

Yang, Huan; Xie, Jiale; Bao, Shu juan; Li, Chang Ming

2015-11-01

Co(OH)2 hollow nanostructures including cube, octahedron and flower are delicately tailored via a simple and fast one-step Cu2O template etching method. The as-prepared materials were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscope (FESEM), N2 adsorption-desorption and electrochemical methods and X-ray photoelectron spectroscopy (XPS). In particular, the supercapacitive behaviors of the as-prepared materials were investigated to explore relation of capacitance versus nanostructure. Results indicate that the as-prepared Co(OH)2 samples inherit the size and shape of the Cu2O templates but with an inside hollow, and the differently nanostructured Co(OH)2 exhibits different capacitive behaviors. Among various morphologies, the flower Co(OH)2 has the largest specific capacitance of 1350 F/g, while octahedron Co(OH)2 has the smallest one of 986.4 F/g. This is mainly because the flower Co(OH)2 not only has the largest available surface area, but also offers the fast interfacial electron transfer for higher pseudocapacitance and enhanced electrolyte ion diffusion rate for high power density, which is supported by both theoretical calculation, measured BET data and ac impedance measurements. This work may provide a vivid example to rationally design a nanostructure and further explore its fundamental insights for high performance supercapacitors. Copyright © 2015 Elsevier Inc. All rights reserved.

Characterization of power induced heating and damage in fiber optic probes for near-field scanning optical microscopy

NASA Astrophysics Data System (ADS)

Dickenson, Nicholas E.; Erickson, Elizabeth S.; Mooren, Olivia L.; Dunn, Robert C.

2007-05-01

Tip-induced sample heating in near-field scanning optical microscopy (NSOM) is studied for fiber optic probes fabricated using the chemical etching technique. To characterize sample heating from etched NSOM probes, the spectra of a thermochromic polymer sample are measured as a function of probe output power, as was previously reported for pulled NSOM probes. The results reveal that sample heating increases rapidly to ˜55-60°C as output powers reach ˜50nW. At higher output powers, the sample heating remains approximately constant up to the maximum power studied of ˜450nW. The sample heating profiles measured for etched NSOM probes are consistent with those previously measured for NSOM probes fabricated using the pulling method. At high powers, both pulled and etched NSOM probes fail as the aluminum coating is damaged. For probes fabricated in our laboratory we find failure occurring at input powers of 3.4±1.7 and 20.7±6.9mW for pulled and etched probes, respectively. The larger half-cone angle for etched probes (˜15° for etched and ˜6° for pulled probes) enables more light delivery and also apparently leads to a different failure mechanism. For pulled NSOM probes, high resolution images of NSOM probes as power is increased reveal the development of stress fractures in the coating at a taper diameter of ˜6μm. These stress fractures, arising from the differential heating expansion of the dielectric and the metal coating, eventually lead to coating removal and probe failure. For etched tips, the absence of clear stress fractures and the pooled morphology of the damaged aluminum coating following failure suggest that thermal damage may cause coating failure, although other mechanisms cannot be ruled out.

Characterization of power induced heating and damage in fiber optic probes for near-field scanning optical microscopy.

PubMed

Dickenson, Nicholas E; Erickson, Elizabeth S; Mooren, Olivia L; Dunn, Robert C

2007-05-01

Tip-induced sample heating in near-field scanning optical microscopy (NSOM) is studied for fiber optic probes fabricated using the chemical etching technique. To characterize sample heating from etched NSOM probes, the spectra of a thermochromic polymer sample are measured as a function of probe output power, as was previously reported for pulled NSOM probes. The results reveal that sample heating increases rapidly to approximately 55-60 degrees C as output powers reach approximately 50 nW. At higher output powers, the sample heating remains approximately constant up to the maximum power studied of approximately 450 nW. The sample heating profiles measured for etched NSOM probes are consistent with those previously measured for NSOM probes fabricated using the pulling method. At high powers, both pulled and etched NSOM probes fail as the aluminum coating is damaged. For probes fabricated in our laboratory we find failure occurring at input powers of 3.4+/-1.7 and 20.7+/-6.9 mW for pulled and etched probes, respectively. The larger half-cone angle for etched probes ( approximately 15 degrees for etched and approximately 6 degrees for pulled probes) enables more light delivery and also apparently leads to a different failure mechanism. For pulled NSOM probes, high resolution images of NSOM probes as power is increased reveal the development of stress fractures in the coating at a taper diameter of approximately 6 microm. These stress fractures, arising from the differential heating expansion of the dielectric and the metal coating, eventually lead to coating removal and probe failure. For etched tips, the absence of clear stress fractures and the pooled morphology of the damaged aluminum coating following failure suggest that thermal damage may cause coating failure, although other mechanisms cannot be ruled out.

Morphological effects of MMPs inhibitors on the dentin bonding

PubMed Central

Li, He; Li, Tianbo; Li, Xiuying; Zhang, Zhimin; Li, Penglian; Li, Zhenling

2015-01-01

Matrix metalloproteinases (MMPs) have been studied extensively, and MMP inhibitors have been used as dental pretreatment agents prior to dentin bonding because they reduce collagen fiber degradation and improve bonding strength. However, morphologic characteristics of the collagen network after etching and of the post-adhesive dentin hybrid layers (DHL) after MMP inhibitors pretreatment have not been evaluated. Thus, we investigated demineralized dentin pretreated with chlorhexidine (CHX) and minocycline (MI) in an etch- and -rinse adhesive system with field emission scanning electron microscopy (FESEM) and immuno-gold labeling markers to observe the collagen network and DHL. FESEM revealed after CHX and MI, a demineralized dentin surface and improved collagen network formation, reduced collagen degradation, and distinct gold-labeling signals. Applying adhesive after either MMP inhibitor created a better dentin interface as evidenced by immuno-gold staining, better adhesive penetration, and higher DHL quality. With microtensile bond strength tests (µTBS) we estimated bonding strength using µTBS data. Immediate µTBS was enhanced with MMP inhibitor application to the bonding surface, and the CHX group was significantly different than non-treated etched surfaces, but no significant change was detected in the MI group. Surface micromorphology of the fractured dentin resin restoration showed that the CHX group had a better resin and dentin tube combination. Both MMP inhibitors created uniform resin coverage. Thus, morphologic results and µTBS data suggest that CHX and MI can inhibit MMP activity, improve immediate bonding strength, and enhance dentin bonding stability with an etch- and -rinse adhesive system. PMID:26379873

Fabrication and Characterization of All-Polystyrene Microfluidic Devices with Integrated Electrodes and Tubing.

PubMed

Pentecost, Amber M; Martin, R Scott

2015-01-01

A new method of fabricating all-polystyrene devices with integrated electrodes and fluidic tubing is described. As opposed to expensive polystyrene (PS) fabrication techniques that use hot embossing and bonding with a heated lab press, this approach involves solvent-based etching of channels and lamination-based bonding of a PS cover, all of which do not need to occur in a clean room. PS has been studied as an alternative microchip substrate to PDMS, as it is more hydrophilic, biologically compatible in terms of cell adhesion, and less prone to absorption of hydrophobic molecules. The etching/lamination-based method described here results in a variety of all-PS devices, with or without electrodes and tubing. To characterize the devices, micrographs of etched channels (straight and intersected channels) were taken using confocal and scanning electron microscopy. Microchip-based electrophoresis with repetitive injections of fluorescein was conducted using a three-sided PS (etched pinched, twin-tee channel) and one-sided PDMS device. Microchip-based flow injection analysis, with dopamine and NO as analytes, was used to characterize the performance of all-PS devices with embedded tubing and electrodes. Limits of detection for dopamine and NO were 130 nM and 1.8 μM, respectively. Cell immobilization studies were also conducted to assess all-PS devices for cellular analysis. This paper demonstrates that these easy to fabricate devices can be attractive alternative to other PS fabrication methods for a wide variety of analytical and cell culture applications.

Effect of tetramethylammonium hydroxide/isopropyl alcohol wet etching on geometry and surface roughness of silicon nanowires fabricated by AFM lithography

PubMed Central

Yusoh, Siti Noorhaniah

2016-01-01

Summary The optimization of etchant parameters in wet etching plays an important role in the fabrication of semiconductor devices. Wet etching of tetramethylammonium hydroxide (TMAH)/isopropyl alcohol (IPA) on silicon nanowires fabricated by AFM lithography is studied herein. TMAH (25 wt %) with different IPA concentrations (0, 10, 20, and 30 vol %) and etching time durations (30, 40, and 50 s) were investigated. The relationships between etching depth and width, and etching rate and surface roughness of silicon nanowires were characterized in detail using atomic force microscopy (AFM). The obtained results indicate that increased IPA concentration in TMAH produced greater width of the silicon nanowires with a smooth surface. It was also observed that the use of a longer etching time causes more unmasked silicon layers to be removed. Importantly, throughout this study, wet etching with optimized parameters can be applied in the design of the devices with excellent performance for many applications. PMID:27826521

Characterization and adsorption properties of diatomaceous earth modified by hydrofluoric acid etching.

PubMed

Tsai, Wen-Tien; Lai, Chi-Wei; Hsien, Kuo-Jong

2006-05-15

This work was a study of the chemical modification of diatomaceous earth (DE) using hydrofluoric acid (HF) solution. Under the experimental conditions investigated, it was found that HF under controlled conditions significantly etched inward into the interior of the existing pore structure in the clay mineral due to its high content of silica, leaving a framework possessing a larger BET surface area (ca. 10 m2 g(-1)) in comparison with that (ca. 4 m2 g(-1)) of its precursor (i.e., DE). Further, the results indicated that the HF concentration is a more determining factor in creating more open pores than other process parameters (temperature, holding time, and solid/liquid ratio). This observation was also in close agreement with the examinations by the silicon analysis, scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. The adsorption kinetics and the adsorption isotherm of methylene blue onto the resulting clay adsorbent can be well described by a pseudo-second-order reaction model and the Freundlich model, respectively.

Lifetime Extension of the Gas Discharge Detectors with Plasma Etching of Silicon Deposits in 80%CF4 + 20%CO2

NASA Astrophysics Data System (ADS)

Gavrilov, G. E.; Vakhtel, V. M.; Maysuzenko, D. A.; Tavtorkina, T. A.; Fetisov, A. A.; Shvetsova, N. Yu.

2017-12-01

A method of elimination of silicon compounds from the anode wire of an aged proportional counter is presented. The aging of a counter with a 70%Ar + 30%CO2 and a 60%Ar + 30%CO2 + 10%CF4 working mixture was stimulated by a 90Sr β source. To accelerate the process of aging, the gas mixture flow to the counter was supplied through a pipe with RTV coated wall. As a result, the amplitude of the signal decreased 70% already at accumulated charge of Q = 0.03 C/cm. The etching of the silicon compounds on the wire surface with an 80%CF4 + 20%CO2 gas mixture discharge led to full recovery of the operating characteristics of detector and an increase in the lifetime. A scanning electron microscopy and X-ray spectroscopy analysis of the recovered wire surface were performed. In accordance with the results, a good quality of wire cleaning from SiO2 compounds was obtained.

Unusual large-pitch banding in poly(L-lactic acid): Effects of composition and geometry confinement

DOE Office of Scientific and Technical Information (OSTI.GOV)

Woo, Eamor M.; Lugito, Graecia; Hsieh, Ya-Ting

2014-02-24

Lamellar patterns and orientations in blends of two crystalline polymers: poly(ethylene oxide) (PEO) and low-molecular-weight poly(L-lactic acid) (PLLA) were investigated using polarizing light optical microscopy (POM), and atomic and scanning electron microscopy (AFM, SEM). Specific etching off of PEO was used to reveal the complex earlier-grown PLLA lamellae patterns with various PEO content in blends. Banding of extremely long pitch (50 μm) in crystallized PLLA spherulites was induced by two kinetic factors: geometry confinement by top cover and introduction of diluent such as PEO. The mechanisms and correlation among the lamellar assembly, ring bands, and cracks are exemplified. Lamellar patternsmore » and ring-band types in blends were found to vary with respect to not only blend compositions, but also confinement of top-cover.« less

Numerical study of bandwidth effect on stimulated Raman backscattering in nonlinear regime

NASA Astrophysics Data System (ADS)

Zhou, H. Y.; Xiao, C. Z.; Zou, D. B.; Li, X. Z.; Yin, Y.; Shao, F. Q.; Zhuo, H. B.

2018-06-01

Nonlinear behaviors of stimulated Raman scattering driven by finite bandwidth pumps are studied by one dimensional particle-in-cell simulations. The broad spectral feature of plasma waves and backscattered light reveals the different coupling and growth mechanisms, which lead to the suppression effect before the deep nonlinear stage. It causes nonperiodic plasma wave packets and reduces packet and etching velocities. Based on the negative frequency shift and electron energy distribution, the long-time evolution of instability can be divided into two stages by the relaxation time. It is a critical time after which the alleviation effects of nonlinear frequency shift and hot electrons are replaced by enhancement. Thus, the broadband pump suppresses instability at early time. However, it aggravates in the deep nonlinear stage by lifting the saturation level due to the coupling of the incident pump with each frequency shifted plasma wave. Our simulation results show that the nonlinear effects are valid in a bandwidth range from 2.25% to 3.0%, and the physics are similar within a nearby parameter space.

Wide angle near-field optical probes by reverse tube etching.

PubMed

Patanè, S; Cefalì, E; Arena, A; Gucciardi, P G; Allegrini, M

2006-04-01

We present a simple modification of the tube etching process for the fabrication of fiber probes for near-field optical microscopy. It increases the taper angle of the probe by a factor of two. The novelty is that the fiber is immersed in hydrofluoric acid and chemically etched in an upside-down geometry. The tip formation occurs inside the micrometer tube cavity formed by the polymeric jacket. By applying this approach, called reverse tube etching, to multimode fibers with 200/250 microm core/cladding diameter, we have fabricated tapered regions featuring high surface smoothness and average cone angles of approximately 30 degrees . A simple model based on the crucial role of the gravity in removing the etching products, explains the tip formation process.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kirtley, John R., E-mail: jkirtley@stanford.edu; Rosenberg, Aaron J.; Palmstrom, Johanna C.

Superconducting QUantum Interference Device (SQUID) microscopy has excellent magnetic field sensitivity, but suffers from modest spatial resolution when compared with other scanning probes. This spatial resolution is determined by both the size of the field sensitive area and the spacing between this area and the sample surface. In this paper we describe scanning SQUID susceptometers that achieve sub-micron spatial resolution while retaining a white noise floor flux sensitivity of ≈2μΦ{sub 0}/Hz{sup 1/2}. This high spatial resolution is accomplished by deep sub-micron feature sizes, well shielded pickup loops fabricated using a planarized process, and a deep etch step that minimizes themore » spacing between the sample surface and the SQUID pickup loop. We describe the design, modeling, fabrication, and testing of these sensors. Although sub-micron spatial resolution has been achieved previously in scanning SQUID sensors, our sensors not only achieve high spatial resolution but also have integrated modulation coils for flux feedback, integrated field coils for susceptibility measurements, and batch processing. They are therefore a generally applicable tool for imaging sample magnetization, currents, and susceptibilities with higher spatial resolution than previous susceptometers.« less

Effect of Different Protocols in Preconditioning With EDTA in Sclerotic Dentin and Enamel Before Universal Adhesives Applied in Self-etch Mode.

PubMed

Martini, E C; Parreiras, S O; Gutierrez, M F; Loguercio, A D; Reis, A

The aim of this study was to investigate the effect of different protocols of 17% ethylene diamine tetra-acetic acid (EDTA) conditioning on the etching pattern and immediate bond strength of universal adhesives to enamel and sclerotic dentin. Forty bovine teeth with sclerotic dentin and 20 human third molars were randomly divided into eight groups resulting from the combination of the main factors surface treatment (none, two-minute EDTA conditioning manual application, 30-second EDTA manual application, 30-second EDTA sonic application) and adhesives systems (Scotchbond Universal Adhesive [SBU] and Prime & Bond Elect [PBE]). Resin-dentin and enamel-dentin bond specimens were prepared and tested under the microtensile bond strength (μTBS) and microshear bond strength (μSBS) tests, respectively. The etching pattern produced on the unground enamel and the sclerotic dentin surfaces under the different protocols and adhesive systems was evaluated under scanning electron microscopy. For enamel, only the main factor adhesive was significant (p<0.0001), with SBU showing the highest μSBS. In sclerotic dentin, the lowest mean was observed for the group without EDTA application and the highest mean in the group with EDTA application with the sonic device for 30 seconds. Regardless of the EDTA protocol, the highest means of μTBS were observed for SBU (p<0.05). EDTA conditioning improves the bonding performance of universal adhesives in the self-etch mode on sclerotic dentin, mainly when applied for 30 seconds with the aid of a sonic device. EDTA pretreatment also improves the retentive etching pattern of enamel, but it does not result in higher enamel bond strength.

Surface pre-treatment of aluminium by cleaning, chemical ething and conversion coating

NASA Astrophysics Data System (ADS)

Zaki, Mohammad Hafizudden Mohd; Mohd, Yusairie; Isa, Nik Norziehana Che

2017-12-01

Surface pre-treatment is one of the critical treatments for surface modification of aluminium (Al). In this study, pre-treatment of Al surface involved three stages; (1) cleaning (polishing and degreasing), (2) chemical etching (alkaline and acid) and (3) conversion coating (ie: zincate treatment). Cleaning process of Al was conducted by polishing and degreasing with acetone while etching process was done by immersion in 1.25 M NaOH solution (i.e: alkaline etching) followed with acid etching using 8 M HNO3 solution. The zincate treatment was conducted via electroless coating method by immersion of Al into a bath solution containing 0.5 M Zn(NO3)2, 0.1 M HNO3 and 0.2 M NaBH4 (reducing agent) for one hour. Different temperatures (ie: 25 °C, 50 °C, 75 °C, 90 °C) of bath solutions at pH 4 were used to investigate the effect of temperature on zincate treatment. Surface morphology and chemical composition of the pre-treated Al were characterized using Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersion X-ray analysis (EDX), respectively. The results showed that oxide layer on Al surface decreased after chemical etching process. Temperature of zincate solution has significantly affected the conversion coating process of aluminium. It was found that zinc oxide (ZnO) and zinc borate (ZnO.B2O3) were dominantly formed after zincate treatment at high temperature (ie:90 °C) with curved blade-like structure and composition of Zn, B and O with 13.70 wt.%, 3.52 wt.% and 54.39 wt.%, respectively. However, zincate treatment at low temperature (ie:<50 °C) has produced low metallic Zn.

Vapor phase diamond growth technology

NASA Technical Reports Server (NTRS)

Angus, J. C.

1981-01-01

Ion beam deposition chambers used for carbon film generation were designed and constructed. Features of the developed equipment include: (1) carbon ion energies down to approx. 50 eV; (2) in suit surface monitoring with HEED; (3) provision for flooding the surface with ultraviolet radiation; (4) infrared laser heating of substrate; (5) residual gas monitoring; (6) provision for several source gases, including diborane for doping studies; and (7) growth from either hydrocarbon source gases or from carbon/argon arc sources. Various analytical techniques for characterization of from carbon/argon arc sources. Various analytical techniques for characterization of the ion deposited carbon films used to establish the nature of the chemical bonding and crystallographic structure of the films are discussed. These include: H2204/HN03 etch; resistance measurements; hardness tests; Fourier transform infrared spectroscopy; scanning auger microscopy; electron spectroscopy for chemical analysis; electron diffraction and energy dispersive X-ray analysis; electron energy loss spectroscopy; density measurements; secondary ion mass spectroscopy; high energy electron diffraction; and electron spin resonance. Results of the tests are summarized.

Silicon etching using only Oxygen at high temperature: An alternative approach to Si micro-machining on 150 mm Si wafers

NASA Astrophysics Data System (ADS)

Chai, Jessica; Walker, Glenn; Wang, Li; Massoubre, David; Tan, Say Hwa; Chaik, Kien; Hold, Leonie; Iacopi, Alan

2015-12-01

Using a combination of low-pressure oxygen and high temperatures, isotropic and anisotropic silicon (Si) etch rates can be controlled up to ten micron per minute. By varying the process conditions, we show that the vertical-to-lateral etch rate ratio can be controlled from 1:1 isotropic etch to 1.8:1 anisotropic. This simple Si etching technique combines the main respective advantages of both wet and dry Si etching techniques such as fast Si etch rate, stiction-free, and high etch rate uniformity across a wafer. In addition, this alternative O2-based Si etching technique has additional advantages not commonly associated with dry etchants such as avoiding the use of halogens and has no toxic by-products, which improves safety and simplifies waste disposal. Furthermore, this process also exhibits very high selectivity (>1000:1) with conventional hard masks such as silicon carbide, silicon dioxide and silicon nitride, enabling deep Si etching. In these initial studies, etch rates as high as 9.2 μm/min could be achieved at 1150 °C. Empirical estimation for the calculation of the etch rate as a function of the feature size and oxygen flow rate are presented and used as proof of concepts.

Enhanced spectroscopic gas sensors using in-situ grown carbon nanotubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

De Luca, A.; Cole, M. T.; Milne, W. I.

2015-05-11

In this letter, we present a fully complementary-metal-oxide-semiconductor (CMOS) compatible microelectromechanical system thermopile infrared (IR) detector employing vertically aligned multi-walled carbon nanotubes (CNT) as an advanced nano-engineered radiation absorbing material. The detector was fabricated using a commercial silicon-on-insulator (SOI) process with tungsten metallization, comprising a silicon thermopile and a tungsten resistive micro-heater, both embedded within a dielectric membrane formed by a deep-reactive ion etch following CMOS processing. In-situ CNT growth on the device was achieved by direct thermal chemical vapour deposition using the integrated micro-heater as a micro-reactor. The growth of the CNT absorption layer was verified through scanning electronmore » microscopy, transmission electron microscopy, and Raman spectroscopy. The functional effects of the nanostructured ad-layer were assessed by comparing CNT-coated thermopiles to uncoated thermopiles. Fourier transform IR spectroscopy showed that the radiation absorbing properties of the CNT adlayer significantly enhanced the absorptivity, compared with the uncoated thermopile, across the IR spectrum (3 μm–15.5 μm). This led to a four-fold amplification of the detected infrared signal (4.26 μm) in a CO{sub 2} non-dispersive-IR gas sensor system. The presence of the CNT layer was shown not to degrade the robustness of the uncoated devices, whilst the 50% modulation depth of the detector was only marginally reduced by 1.5 Hz. Moreover, we find that the 50% normalized absorption angular profile is subsequently more collimated by 8°. Our results demonstrate the viability of a CNT-based SOI CMOS IR sensor for low cost air quality monitoring.« less

Design and synthesis of diverse functional kinked nanowire structures for nanoelectronic bioprobes.

PubMed

Xu, Lin; Jiang, Zhe; Qing, Quan; Mai, Liqiang; Zhang, Qingjie; Lieber, Charles M

2013-02-13

Functional kinked nanowires (KNWs) represent a new class of nanowire building blocks, in which functional devices, for example, nanoscale field-effect transistors (nanoFETs), are encoded in geometrically controlled nanowire superstructures during synthesis. The bottom-up control of both structure and function of KNWs enables construction of spatially isolated point-like nanoelectronic probes that are especially useful for monitoring biological systems where finely tuned feature size and structure are highly desired. Here we present three new types of functional KNWs including (1) the zero-degree KNW structures with two parallel heavily doped arms of U-shaped structures with a nanoFET at the tip of the "U", (2) series multiplexed functional KNW integrating multi-nanoFETs along the arm and at the tips of V-shaped structures, and (3) parallel multiplexed KNWs integrating nanoFETs at the two tips of W-shaped structures. First, U-shaped KNWs were synthesized with separations as small as 650 nm between the parallel arms and used to fabricate three-dimensional nanoFET probes at least 3 times smaller than previous V-shaped designs. In addition, multiple nanoFETs were encoded during synthesis in one of the arms/tip of V-shaped and distinct arms/tips of W-shaped KNWs. These new multiplexed KNW structures were structurally verified by optical and electron microscopy of dopant-selective etched samples and electrically characterized using scanning gate microscopy and transport measurements. The facile design and bottom-up synthesis of these diverse functional KNWs provides a growing toolbox of building blocks for fabricating highly compact and multiplexed three-dimensional nanoprobes for applications in life sciences, including intracellular and deep tissue/cell recordings.

Ion-enhanced chemical etching of ZrO2 in a chlorine discharge

NASA Astrophysics Data System (ADS)

Sha, Lin; Cho, Byeong-Ok; Chang, Jane P.

2002-09-01

Chlorine plasma is found to chemically etch ZrO2 thin films in an electron cyclotron resonance reactor, and the etch rate scaled linearly with the square root of ion energy at high ion energies with a threshold energy between 12-20 eV. The etching rate decreased monotonically with increasing chamber pressures, which corresponds to reduced electron temperatures. Optical emission spectroscopy and quadrupole mass spectrometry were used to identify the reaction etching products. No Zr, O, or ZrCl were detected as etching products, but highly chlorinated zirconium compounds (ZrCl2, ZrCl3, and ZrCl4) and ClO were found to be the dominant etching products. ZrCl3 was the dominant etching products at low ion energies, while ZrCl4 became dominant at higher ion energies. This is consistent with greater momentum transfer and enhanced surface chlorination, as determined by x-ray photoelectron spectroscopy, at increased ion energies. Several ion-enhanced chemical reactions are proposed to contribute to the ZrO2 etching. copyright 2002 American Vacuum Society.

Addition of Grape Seed Extract Renders Phosphoric Acid a Collagen-stabilizing Etchant.

PubMed

Liu, Y; Dusevich, V; Wang, Y

2014-08-01

Previous studies found that grape seed extract (GSE), which is rich in proanthocyanidins, could protect demineralized dentin collagen from collagenolytic activities following clinically relevant treatment. Because of proanthocyanidin's adverse interference to resin polymerization, it was believed that GSE should be applied and then rinsed off in a separate step, which in effect increases the complexity of the bonding procedure. The present study aimed to investigate the feasibility of combining GSE treatment with phosphoric acid etching to address the issue. It is also the first attempt to formulate collagen-cross-linking dental etchants. Based on Fourier-transformed infrared spectroscopy and digestion assay, it was established that in the presence of 20% to 5% phosphoric acid, 30 sec of GSE treatment rendered demineralized dentin collagen inert to bacterial collagenase digestion. Based on this positive result, the simultaneous dentin etching and collagen protecting of GSE-containing phosphoric acid was evaluated on the premise of a 30-second etching time. According to micro-Raman spectroscopy, the formulation containing 20% phosphoric acid was found to lead to overetching. Based on scanning and transmission electronic microscopy, this same formulation exhibited unsynchronized phosphoric acid and GSE penetration. Therefore, addition of GSE did render phosphoric acid a collagen-stabilizing etchant, but the preferable phosphoric acid concentration should be <20%. © International & American Associations for Dental Research.

Fluorescence turn-on sensing of trace cadmium ions based on EDTA-etched CdTe@CdS quantum dot.

PubMed

Wang, Si-Nan; Zhu, Jian; Li, Xin; Li, Jian-Jun; Zhao, Jun-Wu

2018-05-01

Cadmium-caused environmental pollution and diseases have always been worldwide problems. Thus it is extremely urgent to establish a cheap, rapid, simple and selective detection method for trace cadmium in drinking water. In this study, a fluorescence "turn-on" method based on ethylene diamine tetraacetic acid (EDTA)-etched CdTe@CdS quantum dots (QDs) was designed to detect Cd 2+ . High resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) were utilized for chemical and structural characterization of the as-prepared QDs. Based on chemical etching of EDTA on the surface of CdTe@CdS QDs, specific Cd 2+ recognition sites were produced, and then results in fluorescence quenching. The introduction of Cd 2+ could identify these sites and restore the fluorescence of the EDTA-QDs system. Under the optimum conditions, the nanoprobe shows a linear response range from 0.05 to 9 μM with a very low detection limit of 0.032 μM. In addition, the reported fluorescence probe in this work displays a good selectivity for trace Cd 2+ over other metal ions and an admirable practicability in real water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Effects of titanium surface topography on morphology and in vitro activity of human gingival fibroblasts.

PubMed

Ramaglia, L; Capece, G; Di Spigna, G; Bruno, M P; Buonocore, N; Postiglione, L

2013-01-01

The aim of the present study was to evaluate in vitro the biological behavior of human gingival fibroblasts cultured on two different titanium surfaces. Titanium test disks were prepared with a machined, relatively smooth (S) surface or a rough surface (O) obtained by a double acid etching procedure. Primary cultures of human gingival fibroblasts were plated on the experimental titanium disks and cultured up to 14 days. Titanium disk surfaces were analysed by scanning electron microscopy (SEM). Cell proliferation and a quantitative analysis by ELISA in situ of ECM components as CoI, FN and TN were performed. Results have shown different effects of titanium surface microtopography on cell expression and differentiation. At 96 hours of culture on experimental surfaces human gingival fibroblasts displayed a favourable cell attachment and proliferation on both surfaces although showing some differences. Both the relatively smooth and the etched surfaces interacted actively with in vitro cultures of human gingival fibroblasts, promoting cell proliferation and differentiation. Results suggested that the microtopography of a double acid-etched rough surface may induce a greater Co I and FN production, thus conditioning in vivo the biological behaviour of human gingival fibroblasts during the process of peri-implant soft tissue healing.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yue, Mengyao; Zhou, Baoming; Jiao, Kunyan

A switchable surface that promotes either hydrophobic or hydrophilic wettability of poly (L-lactide) (PLLA) microfibrous membranes is obtained by CF₄ microwave plasma treatment in this paper. The results indicated that both etching and grafting process occurred during the CF₄ plasma treatment and these two factors synergistically affected the final surface wettability of PLLA membranes. When plasma treatment was taken under a relatively low power, the surface wettability of PLLA membranes turned from hydrophobic to hydrophilic. Especially when CF₄ plasma treatment was taken under 100 W for 10 min and 150 W for 5 min, the water contact angle sharply decreasedmore » from 116 ± 3.0° to ~0°. According to Field-emission scanning electron microscopy (FESEM) results, the PLLA fibers were notably etched by CF₄ plasma treatment. Combined with the X-ray photoelectron spectroscopy (XPS) measurements, only a few fluorine-containing groups were grafted onto the surface, so the etching effect directly affected the surface wettability of PLLA membranes in low plasma power condition. However, with the plasma power increasing to 200 W, the PLLA membrane surface turned to hydrophobic again. In contrast, the morphology changes of PLLA fiber surfaces were not obvious while a large number of fluorine-containing groups grafted onto the surface. So the grafting effect gradually became the major factor for the final surface wettability.« less

Degradation of Staphylococcus aureus bacteria by neutral oxygen atoms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cvelbar, U.; Mozetic, M.; Hauptman, N.

2009-11-15

The degradation of Staphylococcus aureus bacteria during treatment with neutral oxygen atoms was monitored by scanning electron microscopy. Experiments were performed in an afterglow chamber made from borosilicate glass. The source of oxygen atoms was remote inductively coupled radiofrequency oxygen plasma. The density of atoms at the samples was 8x10{sup 20} m{sup -3}. The treatment was performed at room temperature. The first effect was the removal of dried capsule. Capsule on exposed parts of bacteria was removed after receiving the dose of 6x10{sup 23} at./m{sup 2}, while the parts of capsule filling the gaps between bacteria were removed after receivingmore » the dose of 2.4x10{sup 24} m{sup -2}. After removing the capsule, degradation continued as etching of bacterial cell wall. The etching was rather nonuniform as holes with diameter of several 10 nm were observed. The cell wall was removed after receiving the dose of about 7x10{sup 24} m{sup -2}. The etching probabilities were about 2x10{sup -5} for the capsule and 2x10{sup -6} for the cell wall. The results were explained by different compositions of capsule and the cell wall.« less

Effect of rotary cutting instruments on the resin-tooth interfacial ultra structure: An in vivo study.

PubMed

Sherawat, Sudhir; Tewari, Sanjay; Duhan, Jigyasa; Gupta, Alpa; Singla, Rakesh

2014-12-01

To evaluate the effect of cutting teeth with different types of burs at various speeds on surface topography of tooth surface and interfacial gap formation at resin-tooth interface. The human molars were divided into seven groups: Diamond bur in airrotor (DA) & micromotor (DM), crosscut carbide bur in airrotor (CCA) & micromotor (CCM), plain carbide bur in airrotor (CA) & micromotor (CM) and #600-grit silicon carbide paper (SiC). In five samples from each group Class II box-only cavities were restored. The occlusal surface of four teeth per group was flattened. Two out of four teeth were acid etched. Teeth were subjected for scanning electron microscopy (SEM). Interfacial gap was observed in all groups with no significant difference. SEM observations revealed CA, CCA & DA were coarser than CM, CCM, DM and SiC. SEM of etched tooth surfaces revealed complete removal of amorphous smear layer in CA & CM, partial removal in CCA, CCM, DA & DM and no removal in SiC. Selecting an appropriate bur and its speed may not play an important role in bonding in terms of interfacial gap formation. Variable changes were observed in surface topography with different burs before and after acid etching. Key words:Surface topography, resin-tooth interface, interfacial gap, bonding.

Effect of rotary cutting instruments on the resin-tooth interfacial ultra structure: An in vivo study

PubMed Central

Sherawat, Sudhir; Tewari, Sanjay; Duhan, Jigyasa; Singla, Rakesh

2014-01-01

Objectives: To evaluate the effect of cutting teeth with different types of burs at various speeds on surface topography of tooth surface and interfacial gap formation at resin-tooth interface. Material and Methods: The human molars were divided into seven groups: Diamond bur in airrotor (DA) & micromotor (DM), crosscut carbide bur in airrotor (CCA) & micromotor (CCM), plain carbide bur in airrotor (CA) & micromotor (CM) and #600-grit silicon carbide paper (SiC). In five samples from each group Class II box-only cavities were restored. The occlusal surface of four teeth per group was flattened. Two out of four teeth were acid etched. Teeth were subjected for scanning electron microscopy (SEM). Results: Interfacial gap was observed in all groups with no significant difference. SEM observations revealed CA, CCA & DA were coarser than CM, CCM, DM and SiC. SEM of etched tooth surfaces revealed complete removal of amorphous smear layer in CA & CM, partial removal in CCA, CCM, DA & DM and no removal in SiC. Conclusions: Selecting an appropriate bur and its speed may not play an important role in bonding in terms of interfacial gap formation. Variable changes were observed in surface topography with different burs before and after acid etching. Key words:Surface topography, resin-tooth interface, interfacial gap, bonding. PMID:25674310

Photoluminescent properties of electrochemically synthetized ZnO nanotubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gracia Jiménez, J.M.

ZnO nanotubes were prepared by a sequential combination of electrochemical deposition, chemical attack and regeneration. ZnO nanocolumns were initially electrodeposited on conductive substrates and then converted into nanotubes by a process involving chemical etching and subsequent regrowth. The morphology of these ZnO nanocolumns and derived nanotubes was monitored by Scanning Electron Microscopy and their optical properties was studied by photoluminescence spectroscopy. Photoluminescence were measured as a function of temperature, from 6 to 300 K, for both nanocolumns and nanotubes. In order to study the behaviour of induced intrinsic defect all ZnO films were annealed in air at 400 °C andmore » their photoluminescent properties were also registered before and after annealing. The behaviour of photoluminescence is explained taking into account the contribution of different point defects. A band energy diagram related to intrinsic defects was proposed to describe the behaviour of photoluminescence spectra. - Highlights: •ZnO nanotubes were obtained after etching and regrowth of electrodeposited ZnO films. •Photoluminescence spectra contain two parts involving excitonic and defects transitions. •Annealing produces a blue shift in the PL peaks in both ZnO nanocolumns and nanotubes. •Etching causes a blue shift in PL peaks due to confinement effect in nanotubes walls.« less

Nanoleakage in Hybrid Layer and Acid-Base Resistant Zone at the Adhesive/Dentin Interface.

PubMed

Nikaido, Toru; Nurrohman, Hamid; Takagaki, Tomohiro; Sadr, Alireza; Ichinose, Shizuko; Tagami, Junji

2015-10-01

The aim of interfacial nanoleakage evaluation is to gain a better understanding of degradation of the adhesive-dentin interface. The acid-base resistant zone (ABRZ) is recognized at the bonded interface under the hybrid layer (HL) in self-etch adhesive systems after an acid-base challenge. The purpose of this study was to evaluate nanoleakage in HL and ABRZ using three self-etch adhesives; Clearfil SE Bond (SEB), Clearfil SE One (SEO), and G-Bond Plus (GBP). One of the three adhesives was applied on the ground dentin surface and light cured. The specimens were longitudinally divided into two halves. One half remained as the control group. The others were immersed in ammoniacal silver nitrate solution, followed by photo developing solution under fluorescent light. Following this, the specimens were subjected to acid-base challenges with an artificial demineralization solution (pH4.5) and sodium hypochlorite, and prepared in accordance with common procedures for transmission electron microscopy (TEM) examination. The TEM images revealed silver depositions in HL and ABRZ due to nanoleakage in all the adhesives; however, the extent of nanoleakage was material dependent. Funnel-shaped erosion beneath the ABRZ was observed only in the all-in-one adhesive systems; SEO and GBP, but not in the two-step self-etch adhesive system; SEB.

Magneto-plasmonic nanoparticles as theranostic platforms for magnetic resonance imaging, drug delivery and NIR hyperthermia applications

NASA Astrophysics Data System (ADS)

Urries, Inmaculada; Muñoz, Cristina; Gomez, Leyre; Marquina, Clara; Sebastian, Victor; Arruebo, Manuel; Santamaria, Jesus

2014-07-01

PEGylated magneto-plasmonic nanoparticles with a hollow or semi-hollow interior have been successfully synthesized and their physico-chemical characteristics have been investigated. The hollow interior space can be used to store drugs or other molecules of interest whereas magnetic characterization shows their potential as contrast agents in magnetic resonance imaging (MRI) applications. In addition, their plasmonic characteristics in the near infrared (NIR) region make them efficient in photothermal applications producing high temperature gradients after short irradiation times. We show that by controlling the etching conditions the inner silica shell can be selectively dissolved to achieve a hollow or semi-hollow interior without compromising the magnetic or plasmonic characteristics of the resulting nanoparticles. Magnetic measurements and transmission electron microscopy observations have been used to demonstrate the precise control during the etching process and to select an optimal concentration of the etching reagent and contact time to preserve the inner superparamagnetic iron oxide-based nanoparticles and the plasmonic properties of the constructs. Drug loading capabilities were also evaluated for both semi-hollow and as-synthesized nanoparticles using Rhodamine B isothiocyanate as a model compound. The nanoparticles produced could be potentially used as ``theranostic'' nanoparticles with both imaging capabilities and a dual therapeutic function (drug delivery and hyperthermia).

Magneto-plasmonic nanoparticles as theranostic platforms for magnetic resonance imaging, drug delivery and NIR hyperthermia applications.

PubMed

Urries, Inmaculada; Muñoz, Cristina; Gomez, Leyre; Marquina, Clara; Sebastian, Victor; Arruebo, Manuel; Santamaria, Jesus

2014-08-07

PEGylated magneto-plasmonic nanoparticles with a hollow or semi-hollow interior have been successfully synthesized and their physico-chemical characteristics have been investigated. The hollow interior space can be used to store drugs or other molecules of interest whereas magnetic characterization shows their potential as contrast agents in magnetic resonance imaging (MRI) applications. In addition, their plasmonic characteristics in the near infrared (NIR) region make them efficient in photothermal applications producing high temperature gradients after short irradiation times. We show that by controlling the etching conditions the inner silica shell can be selectively dissolved to achieve a hollow or semi-hollow interior without compromising the magnetic or plasmonic characteristics of the resulting nanoparticles. Magnetic measurements and transmission electron microscopy observations have been used to demonstrate the precise control during the etching process and to select an optimal concentration of the etching reagent and contact time to preserve the inner superparamagnetic iron oxide-based nanoparticles and the plasmonic properties of the constructs. Drug loading capabilities were also evaluated for both semi-hollow and as-synthesized nanoparticles using Rhodamine B isothiocyanate as a model compound. The nanoparticles produced could be potentially used as "theranostic" nanoparticles with both imaging capabilities and a dual therapeutic function (drug delivery and hyperthermia).

Effect of bacterial collagenase on resin-dentin bonds degradation.

PubMed

Toledano, Manuel; Osorio, Raquel; Osorio, Estrella; Aguilera, Fátima S; Yamauti, Monica; Pashley, David H; Tay, Franklin

2007-12-01

The objective of this study is to evaluate the effect of a bacterial collagenase on the degradation of resin-dentin bonds. Human dentin surfaces were bonded with: an etch-&-rinse self-priming adhesive (SB), a two-step self-etching primer/adhesive (SEB), and a 1-step self-etching adhesive (OUB). Composite build-ups were constructed. The bonded teeth were stored (24 h, 3 months, 1 year) in distilled water or in a buffered bacterial collagenase solution. Half of the specimens were stored as intact bonded teeth (Indirect Exposure/IE). The other half were sectioned into beams prior to storage (Direct Exposure/DE). After storage the intact teeth were sectioned into beams and all specimens were tested for microtensile bond strengths (MTBS). ANOVA and multiple comparisons tests were performed. Fractographic analysis was performed by scanning electron microscopy. The inclusion of bacterial collagenase in the storing solution did not lower the MTBS values over those seen in specimens stored in water. SB and SEB bonds strength were equal, and were superior to OUB. After 3 months of DE, SB and OUB bonded specimens showed decreases in MTBS; similar reductions required 1 year for SEB/DE. MTBS did not decrease in IE specimens except for OUB. Resin and collagen dissolution were evident in DE groups after storing.

A review on plasma-etch-process induced damage of HgCdTe

NASA Astrophysics Data System (ADS)

Liu, Lingfeng; Chen, Yiyu; Ye, Zhenhua; Ding, Ruijun

2018-05-01

Dry etching techniques with minimal etch induced damage are required to develop highly anisotropic etch for pixel delineation of HgCdTe infrared focal plane arrays (IRFPAs). High density plasma process has become the main etching technique for HgCdTe in the past twenty years, In this paper, high density plasma electron cyclotron resonance (ECR) and inductively coupled plasma (ICP) etching of HgCdTe are summarized. Common plasma-etch-process induced type conversion and related mechanisms are reviewed particularly.

Evaluation of ASR potential of quartz-rich rocks by alkaline etching of polished rock sections

NASA Astrophysics Data System (ADS)

Šachlová, Šárka; Kuchařová, Aneta; Pertold, Zdeněk; Přikryl, Richard

2015-04-01

Damaging effect of alkali-silica reaction (ASR) on concrete structures has been observed in various countries all over the World. Civil engineers and real state owners are demanding reliable methods in the assessment of ASR potential of aggregates before they are used in constructions. Time feasible methods are expected, as well as methods which enable prediction of long-term behaviour of aggregates in concrete. The most frequently employed accelerated mortar bar test (AMBT) quantifies ASR potential of aggregates according to the expansion values of mortar bars measured after fourteen days testing period. Current study aimed to develop a new methodical approach facilitating identification and quantification of ASR potential of aggregates. Polished rock sections of quartz and amorphous SiO2 (coming from orthoquartzite, quartz meta-greywacke, pegmatite, phyllite, chert, and flint) were subjected to experimental leaching in 1M NaOH solution at 80°C. After 14 days of alkaline etching, the rock sections were analyzed employing scanning electron microscope combined with energy dispersive spectrometer. Representative areas were documented in back scattered electron (BSE) images and measured using fully-automatic petrographic image analysis (PIA). Several features connected to alkaline etching were observed on the surface of polished rock sections: deep alkaline etching, partial leach-out of quartz and amorphous particles, alkaline etching connected to quartz grain boundaries, and alkaline etching without any connection to grain boundaries. All features mentioned above had significant influence on grey-scale spectrum of BSE images. A specific part of the grey-scale spectrum (i.e. grey-shade 0-70) was characteristic of areas affected by alkaline etching (ASR area). By measuring such areas we quantified the extent of alkaline etching in studied samples. Very good correlation was found between the ASR area and ASR potential of investigated rocks measured according to the standard AMBT (folowing ASTM C1260). The etching experiment is regarded to be feasible method to quantify ASR potential of quartz- (resp. SiO2-) rich rocks. Employement of the method: (1) decreases potential error from less experienced operator; (2) minimizes the volume of the rock need to be analyzed; (3) enables to visualize microscopic features where ASR originates; and (4) enables to identify alkali-reactive components in the rocks. The main disadvatage of the method is regarded in the restriction to quartz- (resp. SiO2-) rich rocks. If other minerals are included in the rocks their role in ASR should be considered. These minerals can be excluded from the analysis in case they are not reactive and if their content is very low (e.g. accesory minerals). If the minerals contribute to ASR (e.g. albite, micas), these mineral phases should be included in the analysis. Then the application of PIA needs to be modified in respect to different grey shades of individual minerals.

Influence of the height of the external hexagon and surface treatment on fatigue life of commercially pure titanium dental implants.

PubMed

Gil, Francisco Javier; Aparicio, Conrado; Manero, Jose M; Padros, Alejandro

2009-01-01

This study evaluated the effect of external hexagon height and commonly applied surface treatments on the fatigue life of titanium dental implants. Electropolished commercially pure titanium dental implants (seven implants per group) with three different external hexagon heights (0.6, 1.2, and 1.8 mm) and implants with the highest external hexagon height (1.8 mm) and different surface treatments (electropolishing, grit blasting with aluminium oxide, and acid etching with sulfuric acid) were tested to evaluate their mechanical fatigue life. To do so, 10-Hz triangular flexural load cycles were applied at 37 degrees C in artificial saliva, and the number of load cycles until implant fracture was determined. Tolerances of the hexagon/abutment fit and implant surface roughness were analyzed by scanning electron microscopy and light interferometry. Transmission electron microscopy and electron diffraction analyses of titanium hydrides were performed. First, the fatigue life of implants with the highest hexagon (8,683 +/- 978 load cycles) was more than double that of the implants with the shortest hexagons (3,654 +/- 789 load cycles) (P < .02). Second, the grit-blasted implants had the longest fatigue life of the tested materials (21,393 +/- 2,356 load cycles), which was significantly greater than that of the other surfaces (P < .001). The compressive surface residual stresses induced when blasting titanium are responsible for this superior mechanical response. Third, precipitation of titanium hydrides in grain boundaries of titanium caused by hydrogen adsorption from the acid solution deteriorates the fatigue life of acid-etched titanium dental implants. These implants had the shortest fatigue life (P < .05). The fatigue life of threaded root-form dental implants varies with the height of the external hexagon and/or the surface treatment of the implant. An external hexagon height of 1.8 mm and/or a blasting treatment appear to significantly increase fatigue life of dental implants.

Characterization of Blistering and Delamination in Depleted Uranium Hohlraums

DOE Office of Scientific and Technical Information (OSTI.GOV)

Biobaum, K. J. M.

2013-03-01

Blistering and delamination are the primary failure mechanisms during the processing of depleted uranium (DU) hohlraums. These hohlraums consist of a sputter-deposited DU layer sandwiched between two sputter-deposited layers of gold; a final thick gold layer is electrodeposited on the exterior. The hohlraum is deposited on a copper-coated aluminum mandrel; the Al and Cu are removed with chemical etching after the gold and DU layers are deposited. After the mandrel is removed, blistering and delamination are observed on the interiors of some hohlraums, particularly at the radius region. It is hypothesized that blisters are caused by pinholes in the coppermore » and gold layers; etchant leaking through these holes reaches the DU layer and causes it to oxidize, resulting in a blister. Depending on the residual stress in the deposited layers, blistering can initiate larger-scale delamination at layer interfaces. Scanning electron microscopy indicates that inhomogeneities in the machined aluminum mandrel are replicated in the sputter-deposited copper layer. Furthermore, the Cu layer exhibits columnar growth with pinholes that likely allow etchant to come in contact with the gold layer. Any inhomogeneities or pinholes in this initial gold layer then become nucleation sites for blistering. Using a focused ion beam system to etch through the gold layer and extract a cross-sectional sample for transmission electron microscopy, amorphous, intermixed layers at the gold/DU interfaces are observed. Nanometer-sized bubbles in the sputtered and electrodeposited gold layers are also present. Characterization of the morphology and composition of the deposited layers is the first step in determining modifications to processing parameters, with the goal of attaining a significant improvement in hohlraum yield.« less

Wet-chemical passivation of atomically flat and structured silicon substrates for solar cell application

NASA Astrophysics Data System (ADS)

Angermann, H.; Rappich, J.; Korte, L.; Sieber, I.; Conrad, E.; Schmidt, M.; Hübener, K.; Polte, J.; Hauschild, J.

2008-04-01

Special sequences of wet-chemical oxidation and etching steps were optimised with respect to the etching behaviour of differently oriented silicon to prepare very smooth silicon interfaces with excellent electronic properties on mono- and poly-crystalline substrates. Surface photovoltage (SPV) and photoluminescence (PL) measurements, atomic force microscopy (AFM) and scanning electron microscopy (SEM) investigations were utilised to develop wet-chemical smoothing procedures for atomically flat and structured surfaces, respectively. Hydrogen-termination as well as passivation by wet-chemical oxides were used to inhibit surface contamination and native oxidation during the technological processing. Compared to conventional pre-treatments, significantly lower micro-roughness and densities of surface states were achieved on mono-crystalline Si(100), on evenly distributed atomic steps, such as on vicinal Si(111), on silicon wafers with randomly distributed upside pyramids, and on poly-crystalline EFG ( Edge-defined Film-fed- Growth) silicon substrates. The recombination loss at a-Si:H/c-Si interfaces prepared on c-Si substrates with randomly distributed upside pyramids was markedly reduced by an optimised wet-chemical smoothing procedure, as determined by PL measurements. For amorphous-crystalline hetero-junction solar cells (ZnO/a-Si:H(n)/c-Si(p)/Al) with textured c-Si substrates the smoothening procedure results in a significant increase of short circuit current Isc, fill factor and efficiency η. The scatter in the cell parameters for measurements on different cells is much narrower, as compared to conventional pre-treatments, indicating more well-defined and reproducible surface conditions prior to a-Si:H emitter deposition and/or a higher stability of the c-Si surface against variations in the a-Si:H deposition conditions.

Leucine-rich amelogenin peptide (LRAP) as a surface primer for biomimetic remineralization of superficial enamel defects: An in vitro study.

PubMed

Shafiei, Farhad; Hossein, Bagheri G; Farajollahi, Mohammad M; Fathollah, Moztarzadeh; Marjan, Behroozibakhsh; Tahereh, Jafarzadeh Kashi

2015-01-01

This study was carried out to obtain more information about the assembly of hydroxyapatite bundles formed in the presence of Leucine-Rich Amelogenin Peptide (LRAP) and to evaluate its effect on the remineralization of enamel defects through a biomimetic approach. One or 2 mg/mL LRAP solutions containing 2.5 mM of Ca(+2) and 1.5 mM phosphate were prepared (pH = 7.2) and stored at 37 °C for 24 h. The products of the reaction were studied using atomic force microscopy (AFM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). Vickers surface microhardness recovery (SMR%) of acid-etched bovine enamel, with or without LRAP surface treatment, were calculated to evaluate the influence of peptide on the lesion remineralization. Distilled water and 1 or 2 mg/mL LRAP solution (pH = 7.2) were applied on the lesions and the specimens were incubated in mineralization solution (2.5mM Ca(+2) , 1.5mM PO4 (-3) , pH = 7.2) for 24 h. One-way ANOVA and Tukey's multi-comparison tests were used for statistical analysis. The pattern of enamel surface repair was studied using FE-SEM. AFM showed the formation of highly organized hierarchical structures, composed of hydroxyapatite (HA) crystals, similar to the dental enamel microstructure. ANOVA procedure showed significant effect of peptide treatment on the calculated SMR% (p < 0.001). Tukey's test revealed that peptide treated groups had significantly higher values of SMR%. In conclusion, LRAP is able to regulate the formation of HA and enhances the remineralization of acid-etched enamel as a surface treatment agent. © Wiley Periodicals, Inc.

Influence of Er:YAG and Ti:sapphire laser irradiation on the microtensile bond strength of several adhesives to dentin.

PubMed

Portillo, M; Lorenzo, M C; Moreno, P; García, A; Montero, J; Ceballos, L; Fuentes, M V; Albaladejo, A

2015-02-01

The aim of the present study was to evaluate the influence of erbium:yttrium-aluminum-garnet (Er:YAG) and Ti:sapphire laser irradiation on the microtensile bond strength (MTBS) of three different adhesive systems to dentin. Flat dentin surfaces from 27 molars were divided into three groups according to laser irradiation: control, Er:YAG (2,940 nm, 100 μs, 2.7 W, 9 Hz) and Ti:sapphire laser (795 nm, 120 fs, 1 W, 1 kHz). Each group was divided into three subgroups according to the adhesive system used: two-step total-etching adhesive (Adper Scotchbond 1 XT, from now on XT), two-step self-etching adhesive (Clearfil SE Bond, from now on CSE), and all-in-one self-etching adhesive (Optibond All-in-One, from now on OAO). After 24 h of water storage, beams of section at 1 mm(2) were longitudinally cut from the samples. Each beam underwent traction test in an Instron machine. Fifteen polished dentin specimens were used for the surface morphology analysis by scanning electron microscopy (SEM). Failure modes of representative debonded microbars were SEM-assessed. Data were analyzed by ANOVA, chi-square test, and multiple linear regression (p < 0.05). In the control group, XT obtained higher MTBS than that of laser groups that performed equally. CSE showed higher MTBS without laser than that with laser groups, where Er:YAG attained higher MTBS than ultrashort laser. When OAO was used, MTBS values were equal in the three treatments. CSE obtained the highest MTBS regardless of the surface treatment applied. The Er:YAG and ultrashort laser irradiation reduce the bonding effectiveness when a two-step total-etching adhesive or a two-step self-etching adhesive are used and do not affect their effectiveness when an all-in-one self-etching adhesive is applied.

Matrix metalloproteinase inhibitor modulates esterase-catalyzed degradation of resin-dentin interfaces.

PubMed

Serkies, Kyle B; Garcha, Reena; Tam, Laura E; De Souza, Grace M; Finer, Yoav

2016-12-01

Assess the modulating effect of matrix metalloproteinase (MMP) inhibition on simulated human salivary enzyme (SHSE)-catalyzed degradation of interfacial fracture-toughness (FT) of self-etched and total-etched resin-dentin interfaces. Miniature short-rod FT specimens (N=10/group) containing a resin composite bonded to human dentin, using a self-etch (Easy Bond, EB) or a total-etch (Scotchbond, SB) adhesives, were prepared with and without application of an MMP inhibitor (galardin). Specimens were non-incubated or incubated in phosphate buffered saline (PBS) or SHSE for 7, 30, 90, or 180-days. FT data were obtained using a universal testing machine. Incubation media were analyzed by high performance liquid chromatography (HPLC) for the presence of a 2,2-bis-[4-2(2-hydroxy-3-methacryloxypropoxy)phenyl]-propane (bisGMA)-derived degradation product, bis-hydroxy-propoxy-phenyl-propane (bisHPPP). Fractographic analysis was performed by scanning electron microscopy and image processing software (ImageJ). Statistical analysis was performed by ANOVA and Tukey's (p<0.05). More bisHPPP was detected in SHSE vs. PBS for both adhesive systems (p<0.05). EB specimens yielded no difference in FT and failed preferentially in the resin after >30-days (p<0.05). SB specimens yielded lower FT values after 180-days with SHSE ±galardin vs. 0-days/no-galardin (p<0.05) and failed preferentially in the hybrid-layer after >30-days (p<0.05). Galardin mildly modulated the change in fracture mode for both systems. Esterase-catalyzed degradation of total-etch interfaces is modulated by MMP-inhibition, however, self-etch interfaces possess greater biostability under simulated intra-oral conditions, regardless of MMP inhibition. This could be related to different chemical compositions and/or mode of adhesion. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Scanning electron microscope investigation of the structural growth in thick sputtered coatings

NASA Technical Reports Server (NTRS)

Spalvins, T.

1975-01-01

Sputtered S-Monel, silver, and 304 stainless steel coatings and molybdenum disulfide coatings were deposited on mica and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. The geometry and the surface morphology of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish act as preferential nucleation sites and form isolated overlapping and complex nodules and various unusual surface overgrowths on the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces.

Degradation mechanisms of Ti/Al/Ni/Au-based Ohmic contacts on AlGaN/GaN HEMTs

DOE PAGES

Hwang, Ya-Hsi; Ahn, Shihyun; Dong, Chen; ...

2015-04-27

We investigated the degradation mechanism of Ti/Al/Ni/Au-based Ohmic metallization on AlGaN/GaN high electron mobility transistors upon exposure to buffer oxide etchant (BOE). The major effect of BOE on the Ohmic metal was an increase of sheet resistance from 2.89 to 3.69 Ω/ₜafter 3 min BOE treatment. The alloyed Ohmic metallization consisted 3–5 μm Ni-Al alloy islands surrounded by Au-Al alloy-rings. The morphology of both the islands and ring areas became flatter after BOE etching. Lastly, we used energy dispersive x-ray analysis and Auger electron microscopy to analyze the compositions and metal distributions in the metal alloys prior to and aftermore » BOE exposure.« less

Preparation of mesoporous carbon nitride structure by the dealloying of Ni/a-CN nanocomposite films

NASA Astrophysics Data System (ADS)

Zhou, Han; Shen, Yongqing; Huang, Jie; Liao, Bin; Wu, Xianying; Zhang, Xu

2018-05-01

The preparation of mesoporous carbon nitride (p-CN) structure by the selective dealloying process of Ni/a-CN nanocomposite films is investigated. The composition and structure of the Ni/a-CN nanocomposite films and porous carbon nitride (p-CN) films are determined by scan electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Phase separated structure including nickel carbide phase and the surrounding amorphous carbon nitride (a-CN) matrix are detected for the as-deposited films. Though the bulk diffusion is introduced in the film during the annealing process, the grain sizes for the post-annealed films are around 10 nm and change little comparing with the ones of the as-deposited films, which is associated with the thermostability of the CN surrounding in the film. The p-CN skeleton with its pore size around 12.5 nm is formed by etching the post-annealed films, indicative of the stability of the phase separated structure during the annealing process.

Template-assisted formation of microsized nanocrystalline CeO2 tubes and their catalytic performance in the carboxylation of methanol

PubMed Central

Naumann, Meike; Schäfer, Christian; Brandner, Armin; Hofmann, Heiko J; Claus, Peter

2011-01-01

Summary Polymethylmethacrylate (PMMA)/ceria composite fibres were synthesized by using a sequential combination of polymer electrospinning, spray-coating with a sol, and a final calcination step to yield microstructured ceria tubes, which are composed of nanocrystalline ceria particles. The PMMA template is removed from the organic/inorganic hybrid material by radio frequency (rf) plasma etching followed by calcination of the ceramic green-body fibres. Microsized ceria (CeO2) tubes, with a diameter of ca. 0.75 µm, composed of nanocrystalline agglomerated ceria particles were thus obtained. The 1-D ceramic ceria material was characterized by X-ray diffraction, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), UV–vis and photoluminescence spectroscopy (PL), as well as thermogravimetric analysis (TGA). Its catalytic performance was studied in the direct carboxylation of methanol with carbon dioxide leading to dimethyl carbonate [(CH3O)2CO, DMC], which is widely employed as a phosgene and dimethyl sulfate substitute, and as well as a fuel additive. PMID:22259761

Dimeric arrangement and structure of the membrane-bound acetylcholine receptor studied by electron microscopy.

PubMed Central

Zingsheim, H P; Neugebauer, D C; Frank, J; Hänicke, W; Barrantes, F J

1982-01-01

The acetylcholine receptor protein (AChR) from the electric organ of Torpedo marmorata is studied in its membrane-bound form by electron microscopy and single-particle image averaging. About half the molecule protrudes from the membrane surface by approximately 5 nm. The low-resolution 3-D structure of this hydrated portion, including its handedness, can be deduced from averaged axial and lateral projections and from freeze-etched membrane surfaces. In native membrane fragments, a dimeric form of the AChR is observed and the relative orientation of the AChR monomers within the dimer is established. The dimers disappear upon disulfide reduction of the membrane preparations, whereas the average axial projections of the AChR monomer remain unaffected. Since the existence of disulfide bonds linking AChR monomers between their respective delta-subunits is well documented, the approximate position of the delta-subunit within the low-resolution structure of the AChR molecule can be deduced from the structure of the dimers. Images Fig. 1. Fig. 2. Fig. 3. PMID:7188351

Polymer based nanocomposites with nanofibers and exfoliated clay

NASA Technical Reports Server (NTRS)

Meador, Michael A.; Reneker, Darrell H.

2005-01-01

Polymer solutions, containing clay sheets, were electrospun into nanofibers and microfibers that contained clay sheets inside. Controllable removal of polymer by plasma etching from the surface of fibers revealed the arrangement of clay. The shape, flexibility, size distribution and arrangement of clay sheets were observed by transmission and scanning electron microscopy. The clay sheets were partially aligned in big fibers with normal direction of clay sheets perpendicular to fiber axis. Crumpling of clay sheets inside fibers was observed when the fiber diameter was comparable to the lateral size of clay sheets. Single sheets of clay were observed both by catching clay sheets dispersed in water with electrospun nanofiber mats and by the deliberate removal of most of the polymer in the fibers. Thin, flexible gas barrier films, that are reasonably strong, were assembled from clay sheets and polymer nanofibers. Structure of composite films was characterized with scanning electron microscopy. Continuous film of clay sheets were physically attached to the surface of fiber mats. Spincoating film of polymer and clay sheets was reinforced by electrospun fiber scaffold. Certain alignment of clay sheets was observed in the vicinity of fibers.

Microstructure and mechanical properties of AZ91 magnesium alloy subject to deep cryogenic treatments

NASA Astrophysics Data System (ADS)

Li, Gui-rong; Wang, Hong-ming; Cai, Yun; Zhao, Yu-tao; Wang, Jun-jie; Gill, Simon P. A.

2013-09-01

AZ91 magnesium alloy was subjected to a deep cryogenic treatment. X-ray diffraction (XRD), scanning electronic microscopy (SEM), and transmission electronic microscopy (TEM) methods were utilized to characterize the composition and microstructure of the treated samples. The results show that after two cryogenic treatments, the quantity of the precipitate hardening β phase increases, and the sizes of the precipitates are refined from 8-10 μm to 2-4 μm. This is expected to be due to the decreased solubility of aluminum in the matrix at low temperature and the significant plastic deformation owing to internal differences in thermal contraction between phases and grains. The polycrystalline matrix is also noticeably refined, with the sizes of the subsequent nanocrystalline grains in the range of 50-100 nm. High density dislocations are observed to pile up at the grain boundaries, inducing the dynamic recrystallization of the microstructure, leading to the generation of a nanocrystalline grain structure. After two deep cryogenic treatments, the tensile strength and elongation are found to be substantially increased, rising from 243 MPa and 4.4% of as-cast state to 299 MPa and 5.1%.

Two-step narrow ridge cascade diode lasers emitting near $$2~\\mu$$ m

DOE PAGES

Feng, Tao; Hosoda, Takashi; Shterengas, Leon; ...

2017-01-02

Nearly diffraction limited GaSb-based type-I quantum well cascade diode lasers emitting in the spectral region 1.95-2 μm were designed and fabricated. Two-step 5.5-μm-wide shallow and 14-μm-wide deep etched ridge waveguide design yielded devices generating stable single lobe beams with 250 mW of continuous wave output power at 20 °C. Quantum well radiative recombination current contributes about 13% to laser threshold as estimated from true spontaneous emission and modal gain analysis. Here, recombination at etched sidewalls of the 14-μmwide deep ridges controls about 30% of the threshold.

Compact Submillimeter-Wave Receivers Made with Semiconductor Nano-Fabrication Technologies

NASA Technical Reports Server (NTRS)

Jung, C.; Thomas, B.; Lee, C.; Peralta, A.; Chattopadhyay, G.; Gill, J.; Cooper, K.; Mehdi, I.

2011-01-01

Advanced semiconductor nanofabrication techniques are utilized to design, fabricate and demonstrate a super-compact, low-mass (<10 grams) submillimeter-wave heterodyne front-end. RF elements such as waveguides and channels are fabricated in a silicon wafer substrate using deep-reactive ion etching (DRIE). Etched patterns with sidewalls angles controlled with 1 deg precision are reported, while maintaining a surface roughness of better than 20 nm rms for the etched structures. This approach is being developed to build compact 2-D imaging arrays in the THz frequency range.

Electron-beam induced nano-etching of suspended graphene

PubMed Central

Sommer, Benedikt; Sonntag, Jens; Ganczarczyk, Arkadius; Braam, Daniel; Prinz, Günther; Lorke, Axel; Geller, Martin

2015-01-01

Besides its interesting physical properties, graphene as a two-dimensional lattice of carbon atoms promises to realize devices with exceptional electronic properties, where freely suspended graphene without contact to any substrate is the ultimate, truly two-dimensional system. The practical realization of nano-devices from suspended graphene, however, relies heavily on finding a structuring method which is minimally invasive. Here, we report on the first electron beam-induced nano-etching of suspended graphene and demonstrate high-resolution etching down to ~7 nm for line-cuts into the monolayer graphene. We investigate the structural quality of the etched graphene layer using two-dimensional (2D) Raman maps and demonstrate its high electronic quality in a nano-device: A 25 nm-wide suspended graphene nanoribbon (GNR) that shows a transport gap with a corresponding energy of ~60 meV. This is an important step towards fast and reliable patterning of suspended graphene for future ballistic transport, nano-electronic and nano-mechanical devices. PMID:25586495

The effect of Er:YAG laser irradiation on the bond stability of self-etch adhesives at different dentin depths.

PubMed

Karadas, Muhammet; Çağlar, İpek

2017-07-01

The aim of this study was to evaluate the effect of Er:YAG laser irradiation on the micro-shear bond strength of self-etch adhesives to the superficial dentin and the deep dentin before and after thermocycling. Superficial dentin and deep dentin surfaces were prepared by flattening of the occlusal surfaces of extracted human third molars. The deep or superficial dentin specimens were randomized into three groups according to the following surface treatments: group I (control group), group II (Er:YAG laser; 1.2 W), and group III (Er:YAG laser; 0.5 W). Clearfil SE Bond or Clearfil S 3 Bond was applied to each group's dentin surfaces. After construction of the composite blocks on the dentin surface, the micro-shear bond testing of each adhesive was performed at 24 h or after 15,000 thermal cycles. The data were analyzed using a univariate analysis of variance and Tukey's test (p < 0.05). Laser irradiation in superficial dentin did not significantly affect bond strength after thermocycling (p > 0.05). However, deep-dentin specimens irradiated with laser showed significantly higher bond strengths than did control specimens after thermocycling (p < 0.05). Thermocycling led to significant deterioration in the bond strengths of all deep-dentin groups. The stable bond strength after thermocycling was measured for all of the superficial-dentin groups. No significant difference was found between the 0.5 and 1.2 W output power settings. In conclusion, the effect of laser irradiation on the bond strength of self-etch adhesives may be altered by the dentin depth. Regardless of the applied surface treatment, deep dentin showed significant bond degradation.

Correlating Intravital Multi-Photon Microscopy to 3D Electron Microscopy of Invading Tumor Cells Using Anatomical Reference Points

PubMed Central

Karreman, Matthia A.; Mercier, Luc; Schieber, Nicole L.; Shibue, Tsukasa; Schwab, Yannick; Goetz, Jacky G.

2014-01-01

Correlative microscopy combines the advantages of both light and electron microscopy to enable imaging of rare and transient events at high resolution. Performing correlative microscopy in complex and bulky samples such as an entire living organism is a time-consuming and error-prone task. Here, we investigate correlative methods that rely on the use of artificial and endogenous structural features of the sample as reference points for correlating intravital fluorescence microscopy and electron microscopy. To investigate tumor cell behavior in vivo with ultrastructural accuracy, a reliable approach is needed to retrieve single tumor cells imaged deep within the tissue. For this purpose, fluorescently labeled tumor cells were subcutaneously injected into a mouse ear and imaged using two-photon-excitation microscopy. Using near-infrared branding, the position of the imaged area within the sample was labeled at the skin level, allowing for its precise recollection. Following sample preparation for electron microscopy, concerted usage of the artificial branding and anatomical landmarks enables targeting and approaching the cells of interest while serial sectioning through the specimen. We describe here three procedures showing how three-dimensional (3D) mapping of structural features in the tissue can be exploited to accurately correlate between the two imaging modalities, without having to rely on the use of artificially introduced markers of the region of interest. The methods employed here facilitate the link between intravital and nanoscale imaging of invasive tumor cells, enabling correlating function to structure in the study of tumor invasion and metastasis. PMID:25479106

New Methods of Sample Preparation for Atom Probe Specimens

NASA Technical Reports Server (NTRS)

Kuhlman, Kimberly, R.; Kowalczyk, Robert S.; Ward, Jennifer R.; Wishard, James L.; Martens, Richard L.; Kelly, Thomas F.

2003-01-01

Magnetite is a common conductive mineral found on Earth and Mars. Disk-shaped precipitates approximately 40 nm in diameter have been shown to have manganese and aluminum concentrations. Atom-probe field-ion microscopy (APFIM) is the only technique that can potentially quantify the composition of these precipitates. APFIM will be used to characterize geological and planetary materials, analyze samples of interest for geomicrobiology; and, for the metrology of nanoscale instrumentation. Prior to APFIM sample preparation was conducted by electropolishing, the method of sharp shards (MSS), or Bosch process (deep reactive ion etching) with focused ion beam (FIB) milling as a final step. However, new methods are required for difficult samples. Many materials are not easily fabricated using electropolishing, MSS, or the Bosch process, FIB milling is slow and expensive, and wet chemistry and the reactive ion etching are typically limited to Si and other semiconductors. APFIM sample preparation using the dicing saw is commonly used to section semiconductor wafers into individual devices following manufacture. The dicing saw is a time-effective method for preparing high aspect ratio posts of poorly conducting materials. Femtosecond laser micromachining is also suitable for preparation of posts. FIB time required is reduced by about a factor of 10 and multi-tip specimens can easily be fabricated using the dicing saw.

Diversity of life in ocean floor basalt

NASA Astrophysics Data System (ADS)

Thorseth, I. H.; Torsvik, T.; Torsvik, V.; Daae, F. L.; Pedersen, R. B.

2001-12-01

Electron microscopy and biomolecular methods have been used to describe and identify microbial communities inhabiting the glassy margins of ocean floor basalts. The investigated samples were collected from a neovolcanic ridge and from older, sediment-covered lava flows in the rift valley of the Knipovich Ridge at a water depth around 3500 m and an ambient seawater temperature of -0.7°C. Successive stages from incipient microbial colonisation, to well-developed biofilms occur on fracture surfaces in the glassy margins. Observed microbial morphologies are various filamentous, coccoidal, oval, rod-shaped and stalked forms. Etch marks in the fresh glass, with form and size resembling the attached microbes, are common. Precipitation of alteration products around microbes has developed hollow subspherical and filamentous structures. These precipitates are often enriched in Fe and Mn. The presence of branching and twisted stalks that resemble those of the iron-oxidising Gallionella, indicate that reduced iron may be utilised in an energy metabolic process. Analysis of 16S-rRNA gene sequences from microbes present in the rock samples, show that the bacterial population inhabiting these samples cluster within the γ- and ɛ-Proteobacteria and the Cytophaga/Flexibacter/Bacteroides subdivision of the Bacteria, while the Archaea all belong to the Crenarchaeota kingdom. This microbial population appears to be characteristic for the rock and their closest relatives have previously been reported from cold marine waters in the Arctic and Antarctic, deep-sea sediments and hydrothermal environments.

The influence of temporary cements on dental adhesive systems for luting cementation.

PubMed

Ribeiro, José C V; Coelho, Paulo G; Janal, Malvin N; Silva, Nelson R F A; Monteiro, André J; Fernandes, Carlos A O

2011-03-01

This study tested the hypothesis that bond strength of total- and self-etching adhesive systems to dentine is not affected by the presence of remnants from either eugenol-containing (EC) or eugenol-free (EF) temporary cements after standardized cleaning procedures. Thirty non-carious human third molars were polished flat to expose dentine surfaces. Provisional acrylic plates were fabricated and cemented either with EC, EF or no temporary cements. All specimens were incubated for 7 days in water at 37°C. The restorations were then taken out and the remnants of temporary cements were mechanically removed with a dental instrument. The dentine surfaces were cleaned with pumice and treated with either total-etching (TE) or self-etching (SE) dental adhesive systems. Atomic force microscopy was used to examine the presence of remnants of temporary cements before and after dentine cleaning procedures. Composite resin build-ups were fabricated and cemented to the bonded dentine surfaces with a resin luting cement. The specimens were then sectioned to obtain 0.9mm(2) beams for microtensile bond strength testing. Fractographic analysis was performed by optical and scanning electron microscopy. ANOVA showed lower mean microtensile bond strength in groups of specimens treated with EC temporary cement than in groups treated with either no cement or an EF cement (p<0.05). Mean microtensile bond strength was lower in groups employing the SE rather than the TE adhesive system (p<0.001). SE samples were also more likely to fail during initial processing of the samples. There was no evidence of interaction between cement and adhesive system effects on tensile strength. Fractographic analysis indicated different primary failure modes for SE and TE bonding systems, at the dentine-adhesive interface and at the resin cement-resin composite interface, respectively. The use of eugenol-containing temporary cements prior to indirect bonding restorations reduce, to a statistically similar extent, the bond strength of both total- and self-etching adhesive systems to dentine. Copyright © 2011 Elsevier Ltd. All rights reserved.

Big Data and Deep data in scanning and electron microscopies: functionality from multidimensional data sets

DOE PAGES

Belianinov, Alex; Vasudevan, Rama K; Strelcov, Evgheni; ...

2015-05-13

The development of electron, and scanning probe microscopies in the second half of the twentieth century have produced spectacular images of internal structure and composition of matter with, at nanometer, molecular, and atomic resolution. Largely, this progress was enabled by computer-assisted methods of microscope operation, data acquisition and analysis. The progress in imaging technologies in the beginning of the twenty first century has opened the proverbial floodgates of high-veracity information on structure and functionality. High resolution imaging now allows information on atomic positions with picometer precision, allowing for quantitative measurements of individual bond length and angles. Functional imaging often leadsmore » to multidimensional data sets containing partial or full information on properties of interest, acquired as a function of multiple parameters (time, temperature, or other external stimuli). Here, we review several recent applications of the big and deep data analysis methods to visualize, compress, and translate this data into physically and chemically relevant information from imaging data.« less

Big Data and Deep data in scanning and electron microscopies: functionality from multidimensional data sets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Belianinov, Alex; Vasudevan, Rama K; Strelcov, Evgheni

The development of electron, and scanning probe microscopies in the second half of the twentieth century have produced spectacular images of internal structure and composition of matter with, at nanometer, molecular, and atomic resolution. Largely, this progress was enabled by computer-assisted methods of microscope operation, data acquisition and analysis. The progress in imaging technologies in the beginning of the twenty first century has opened the proverbial floodgates of high-veracity information on structure and functionality. High resolution imaging now allows information on atomic positions with picometer precision, allowing for quantitative measurements of individual bond length and angles. Functional imaging often leadsmore » to multidimensional data sets containing partial or full information on properties of interest, acquired as a function of multiple parameters (time, temperature, or other external stimuli). Here, we review several recent applications of the big and deep data analysis methods to visualize, compress, and translate this data into physically and chemically relevant information from imaging data.« less

Flexible deep brain neural probes based on a parylene tube structure

NASA Astrophysics Data System (ADS)

Zhao, Zhiguo; Kim, Eric; Luo, Hao; Zhang, Jinsheng; Xu, Yong

2018-01-01

Most microfabricated neural probes have limited shank length, which prevents them from reaching many deep brain structures. This paper reports deep brain neural probes with ultra-long penetrating shanks based on a simple but novel parylene tube structure. The mechanical strength of the parylene tube shank is temporarily enhanced during implantation by inserting a metal wire. The metal wire can be removed after implantation, making the implanted probe very flexible and thus minimizing the stress caused by micromotions of brain tissues. Optogenetic stimulation and chemical delivery capabilities can be potentially integrated by taking advantage of the tube structure. Single-shank prototypes with a shank length of 18.2 mm have been developed. The microfabrication process comprises of deep reactive ion etching (DRIE) of silicon, parylene conformal coating/refilling, and XeF2 isotropic silicon etching. In addition to bench-top insertion characterization, the functionality of developed probes has been preliminarily demonstrated by implanting into the amygdala of a rat and recording neural signals.

Deep Eutectic Solvent Synthesis of LiMnPO4/C Nanorods as a Cathode Material for Lithium Ion Batteries

PubMed Central

Wu, Zhi; Huang, Rong-Rong; Yu, Hang; Xie, Yong-Chun; Lv, Xiao-Yan; Su, Jing; Long, Yun-Fei; Wen, Yan-Xuan

2017-01-01

Olivine-type LiMnPO4/C nanorods were successfully synthesized in a chloride/ethylene glycol-based deep eutectic solvent (DES) at 130 °C for 4 h under atmospheric pressure. As-synthesized samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR) and electrochemical tests. The prepared LiMnPO4/C nanorods were coated with a thin carbon layer (approximately 3 nm thick) on the surface and had a length of 100–150 nm and a diameter of 40–55 nm. The prepared rod-like LiMnPO4/C delivered a discharge capacity of 128 mAh·g−1 with a capacity retention ratio of approximately 93% after 100 cycles at 1 C. Even at 5 C, it still had a discharge capacity of 106 mAh·g−1, thus exhibiting good rate performance and cycle stability. These results demonstrate that the chloride/ethylene glycol-based deep eutectic solvents (DES) can act as a new crystal-face inhibitor to adjust the oriented growth and morphology of LiMnPO4. Furthermore, deep eutectic solvents provide a new approach in which to control the size and morphology of the particles, which has a wide application in the synthesis of electrode materials with special morphology. PMID:28772493

Deep Eutectic Solvent Synthesis of LiMnPO₄/C Nanorods as a Cathode Material for Lithium Ion Batteries.

PubMed

Wu, Zhi; Huang, Rong-Rong; Yu, Hang; Xie, Yong-Chun; Lv, Xiao-Yan; Su, Jing; Long, Yun-Fei; Wen, Yan-Xuan

2017-02-06

Olivine-type LiMnPO₄/C nanorods were successfully synthesized in a chloride/ethylene glycol-based deep eutectic solvent (DES) at 130 °C for 4 h under atmospheric pressure. As-synthesized samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR) and electrochemical tests. The prepared LiMnPO₄/C nanorods were coated with a thin carbon layer (approximately 3 nm thick) on the surface and had a length of 100-150 nm and a diameter of 40-55 nm. The prepared rod-like LiMnPO₄/C delivered a discharge capacity of 128 mAh·g -1 with a capacity retention ratio of approximately 93% after 100 cycles at 1 C. Even at 5 C, it still had a discharge capacity of 106 mAh·g -1 , thus exhibiting good rate performance and cycle stability. These results demonstrate that the chloride/ethylene glycol-based deep eutectic solvents (DES) can act as a new crystal-face inhibitor to adjust the oriented growth and morphology of LiMnPO₄. Furthermore, deep eutectic solvents provide a new approach in which to control the size and morphology of the particles, which has a wide application in the synthesis of electrode materials with special morphology.

Stability of field emission current from porous n-GaAs(110)

NASA Astrophysics Data System (ADS)

Tondare, V. N.; Naddaf, M.; Bhise, A. B.; Bhoraskar, S. V.; Joag, D. S.; Mandale, A. B.; Sainkar, S. R.

2002-02-01

Field electron emission from porous GaAs has been investigated. The emitter was prepared by anodic etching of n-GaAs (110) in 0.1 M HCl solution. The as-etched porous GaAs shows nonlinear Fowler-Nordheim (FN) characteristics, with a low onset voltage. The emitter, after operating for 6 h at the residual gas pressure of 1×10-8 mbar, shows a linear FN characteristics with a relatively high onset voltage and poor field emission current stability as compared to the as-etched emitter. The change in the behavior was attributed to the residual gas ion bombardment during field electron emission. X-ray photoelectron spectroscopic investigations were carried out on as-etched sample and the one which was studied for field emission. The studies indicate that the as-etched surface contains As2O3 and the surface after field electron emission for about 6 h becomes gallium rich. The presence of As2O3 seems to be a desirable feature for the stable field emission current.

Electronic-carrier-controlled photochemical etching process in semiconductor device fabrication

DOEpatents

Ashby, C.I.H.; Myers, D.R.; Vook, F.L.

1988-06-16

An electronic-carrier-controlled photochemical etching process for carrying out patterning and selective removing of material in semiconductor device fabrication includes the steps of selective ion implanting, photochemical dry etching, and thermal annealing, in that order. In the selective ion implanting step, regions of the semiconductor material in a desired pattern are damaged and the remainder of the regions of the material not implanted are left undamaged. The rate of recombination of electrons and holes is increased in the damaged regions of the pattern compared to undamaged regions. In the photochemical dry etching step which follows ion implanting step, the material in the undamaged regions of the semiconductor are removed substantially faster than in the damaged regions representing the pattern, leaving the ion-implanted, damaged regions as raised surface structures on the semiconductor material. After completion of photochemical dry etching step, the thermal annealing step is used to restore the electrical conductivity of the damaged regions of the semiconductor material.

Electronic-carrier-controlled photochemical etching process in semiconductor device fabrication

DOEpatents

Ashby, Carol I. H.; Myers, David R.; Vook, Frederick L.

1989-01-01

An electronic-carrier-controlled photochemical etching process for carrying out patterning and selective removing of material in semiconductor device fabrication includes the steps of selective ion implanting, photochemical dry etching, and thermal annealing, in that order. In the selective ion implanting step, regions of the semiconductor material in a desired pattern are damaged and the remainder of the regions of the material not implanted are left undamaged. The rate of recombination of electrons and holes is increased in the damaged regions of the pattern compared to undamaged regions. In the photochemical dry etching step which follows ion implanting step, the material in the undamaged regions of the semiconductor are removed substantially faster than in the damaged regions representing the pattern, leaving the ion-implanted, damaged regions as raised surface structures on the semiconductor material. After completion of photochemical dry etching step, the thermal annealing step is used to restore the electrical conductivity of the damaged regions of the semiconductor material.

Effect of different atmospheres on the electrical contact performance of electronic components under fretting wear

NASA Astrophysics Data System (ADS)

Liu, Xin-Long; Cai, Zhen-Bing; Cui, Ye; Liu, Shan-Bang; Xu, Xiao-Jun; Zhu, Min-Hao

2018-04-01

The effects of oxide etch on the surface morphology of metals for industrial application is a common cause of electrical contacts failure, and it has becomes a more severe problem with the miniaturization of modern electronic devices. This study investigated the effects of electrical contact resistance on the contactor under three different atmospheres (oxygen, air, and nitrogen) based on 99.9% copper/pogo pins contacts through fretting experiments. The results showed the minimum and stable electrical contact resistance value when shrouded in the nitrogen environment and with high friction coefficient. The rich oxygen environment promotes the formation of cuprous oxide, thereby the electrical contact resistance increases. Scanning electron microscope microscopy and electron probe microanalysis were used to analyze the morphology and distribution of elements of the wear area, respectively. The surface product between contacts was investigated by x-ray photoelectron spectroscopy analysis to explain the different electrical contact properties of the three tested samples during fretting.

Synthesis of Graphene Based Membranes: Effect of Substrate Surface Properties on Monolayer Graphene Transfer.

PubMed

Kafiah, Feras; Khan, Zafarullah; Ibrahim, Ahmed; Atieh, Muataz; Laoui, Tahar

2017-01-21

In this work, we report the transfer of graphene onto eight commercial microfiltration substrates having different pore sizes and surface characteristics. Monolayer graphene grown on copper by the chemical vapor deposition (CVD) process was transferred by the pressing method over the target substrates, followed by wet etching of copper to obtain monolayer graphene/polymer membranes. Scanning electron microscopy (SEM), atomic force microscopy (AFM), and contact angle (CA) measurements were carried out to explore the graphene layer transferability. Three factors, namely, the substrate roughness, its pore size, and its surface wetting (degree of hydrophobicity) are found to affect the conformality and coverage of the transferred graphene monolayer on the substrate surface. A good quality graphene transfer is achieved on the substrate with the following characteristics; being hydrophobic (CA > 90°), having small pore size, and low surface roughness, with a CA to RMS (root mean square) ratio higher than 2.7°/nm.