Toward local growth of individual nanowires on three-dimensional microstructures by using a minimally invasive catalyst templating method

We present a novel minimally invasive postprocessing method for catalyst templating based on focused charged particle beam structuring, which enables a localized vapor-liquid-solid (VLS) growth of individual nanowires on prefabricated three-dimensional micro- and nanostructures. Gas-assisted focused electron beam induced deposition (FEBID) was used to deposit a SiO(x) surface layer of about 10 × 10 μm(2) on top of a silicon atomic force microscopy cantilever. Gallium focused ion beam (FIB) milling was used to make a hole through the SiO(x) layer into the underlying silicon. The hole was locally filled with a gold catalyst via FEBID using either Me(2)Au(tfac) or Me(2)Au(acac) as precursor. Subsequent chemical vapor deposition (CVD)-induced VLS growth using a mixture of SiH(4) and Ar resulted in individual high quality crystalline nanowires. The process, its yield, and the resulting angular distribution/crystal orientation of the silicon nanowires are discussed. The presented combined FIB/FEBID/CVD-VLS process is currently the only proven method that enables the growth of individual monocrystalline Si nanowires on prestructured substrates and devices.     

Dual-Color InAs/GaSb Superlattice Focal-Plane Array Technology

Within a very few years, InAs/GaSb superlattice technology has proven its suitability for high-performance infrared imaging detector arrays. At the Fraunhofer Institute for Applied Solid State Physics (IAF) and AIM Infrarot-Module GmbH, efforts have been focused on developing mature fabrication technology for dual-color InAs/GaSb superlattice focal-plane arrays for simultaneous, colocated detection at 3 μm to 4 μm and 4 μm to 5 μm in the mid-wavelength infrared atmospheric transmission window. Integrated into a wide-field-of-view missile approach warning system for an airborne platform, a very low number of pixel outages and cluster defects is mandatory for bispectral detector arrays. Process refinements, intense root-cause analysis, and specific test methodologies employed at various stages during the process have proven to be the key for yield enhancements.     

Inorganic and organic arsenic in some commercial east australian crustacea

The levels of inorganic and organic arsenic have been determined in a total of 86 samples of crustacea which included School prawns (Metapenaeus macleayi), King prawns (Penaeus plebejus), Royal Red prawns (Hymenopenaeus sibogae), Eastern Common crayfish (Jasus verreauxii), Blue Swimmer crab (Portunus pelagicus) and Mud crab (Scylla serrata). Most samples were obtained from New South Wales coastal waters and the remainder were purchased at the Sydney fish markets. Inorganic arsenic was isolated by distillation as the chloride and determined by an atomic absorption-hydride generation method. Organic arsenic was determined on the remaining solution by flame atomic absorption spectrophotometry after digestion of the organic matter with a mixture of nitric, perchloric and sulphuric acids (25 + 5 +1). The Eastern Common crayfish contained the highest levels of inorganic and organic arsenic with ranges of 0.12–0.41 mg kg^?1 and 11.9–54.1 mg kg^?1 (wet basis), respectively. Of the remaining samples, 85% contained inorganic arsenic at <0.1 mg kg^?1 and 97% contained organic arsenic at <7 mg kg^?1. The absolute sensitivity and detection limit of the inorganic arsenic method was estimated to be 3 ng (0.03 mg kg^?1). For the organic arsenic method the sensitivity and detection limits were estimated as 0.5 and 0.8 mg kg^?1, respectively.     

Mechanism of formation of urchin-like ZnO

Thin films composed of ZnO nanowires (NWs) hierarchically organized with an urchin-like 3D morphology were obtained by combining the electrochemical deposition and sphere lithography methods. Deposited on a transparent conductive oxide substrate (TCO), a monolayer of carboxylate modified polystyrene spheres organized with a hexagonal closed-packed structure played the role of a template. The spheres were activated in a solution of zinc chloride by the formation of bonds between the carboxylate terminals and the Zn²⁺ ions and were used as a template for the electrodeposition of vertically aligned ZnO NWs around them. Without this treatment, ZnO NWs were deposited only on the TCO substrate between the PS spheres. To reach a density of nanowires high enough to obtain the urchin morphology, the concentration of ZnCl₂ had to be at least equal to 2 M. It was also found, as soon as small grains of ZnO started to be electrodeposited on the polystyrene spheres that the spheres were no longer close packed. The space created between them increased with the increase in the number of small ZnO grains and the increase in their length, allowing the further growth of the nanowires between the spheres. As a result the initial round shape of the spheres was modified and the urchin-like ZnO exhibited an ellipsoidal shape.     

Effect of high temperature and the role of sulfate on adsorption behavior and effectiveness of AMPS®‐based cement fluid loss polymers

The fluid loss control performance of 2‐acrylamido‐2‐methylpropane sulfonic acid (AMPS®)‐based copolymers added to cement slurries was studied at 27 and 100°C, respectively. It was found that effectiveness of these fluid loss additives solely relies on achievement of a high adsorbed amount on the surface of cement. At elevated temperature (100°C), CaAMPS®‐N,N‐dimethyl acrylamide copolymer (CaAMPS®‐co‐NNDMA) exhibits reduced adsorption and hence decreased fluid loss control of the cement slurry. The reason behind this behavior is poor calcium binding capability of the sulfonate anchor groups, which coordinate with calcium atoms present on the mineral surface. Whereas, an increase in the sulfate concentration present in cement pore solution instigates partial coiling of CaAMPS®‐co‐NNDMA and causes only a slight influence on the performance of this copolymer. The elevated sulfate content results from thermal degradation of ettringite, a cement hydrate mineral produced during the early stages of cement hydration. Incorporation of minor amounts (～ 1.3 mol %) of maleic anhydride into this copolymer produces a terpolymer, which exhibits higher and more stable adsorption, even at high temperature. This effect is owed to the presence of homopolymer blocks of polycarboxylates distributed along the polymer trunk. On mineral surfaces, they present much stronger anchor groups than sulfonate functionalities, as evidenced by their higher calcium binding capability. Consequently, fluid loss performance of CaAMPS®‐co‐NNDMA‐co‐MA is little affected by temperature. Understanding the influence of temperature on the physicochemical interactions occurring between additives and the mineral surface can help to design more effective admixtures suitable for high temperature applications. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Polyelectrolyte complexes from polyethylene imine/acetone formaldehyde sulfite polycondensates: A novel reagent for effective fluid loss control of oil well cement slurries

When used by itself, polyethylene imine (PEI) does not perform well as cement fluid loss additive. Its combination with acetone formaldehyde sulfite (AFS) polycondensate, however, exhibits excellent filtration control. The mechanism underlying this synergistic effect was studied and the conditions producing best results were determined. For optimum performance, PEI and AFS must be reacted with each other to yield a polyelectrolyte complex (PEC) (d ～ 5–10 μm), which effectively plugs the pores of the cement filter cake. Composition, size, and effectiveness of the PEC are strongly influenced by the anionic charge amount of the AFS dispersant. Ionic interactions between cationic imine functionalities of PEI and anionic sulfonate groups existing in AFS were confirmed by conductivity, infrared, zeta potential, and particle size measurements. For AFS samples possessing different degrees of sulfonation, the largest particle size and hence best fluid loss performance of the PEC was found to occur at a PEI:AFS molar ratio, which corresponds to neutral charge. Occurrence of large PEC particles (d ～ 5 μm) within the cement filter cake pores was visualized by scanning electron microscopy, and their stability in highly alkaline cement pore solution was confirmed by particle size measurement. Other anionic polyelectrolytes may be used to yield such PECs with PEI to provide effective fluid loss control for cement slurries. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Simultaneous determination of type A,B and D trichothecenes and their occurrence in cereals and cereal products

A sensitive LC–MS/MS method for the simultaneous determination of type A, B and D trichothecenes in cereals is presented. The limits of detection ranged between 0.1 and 0.7 µg kg^?1 for all analytes. The method was applied to 289 representatively drawn samples of wheat, rye and oat products. Ninety-four percent of the wheat samples (n = 130), 95% of the rye samples (n = 61) and 100% of the oat samples (n = 98) were contaminated with the type A trichothecenes T-2 and HT-2 toxin. Median levels of T-2/HT-2 (sum of the toxins) were 0.91, 0.53 and 8.2 µg kg^?1, respectively. Highest levels were found in wheat bran (24 µg kg^?1), rye kernels (3.1 µg kg^?1) and oat flakes (85 µg kg^?1). All wheat and rye samples and 75% of the oat samples were contaminated with the type B trichothecene deoxynivalenol. Median levels of this toxin were 23, 15 and 0.53 µg kg^?1, respectively. Highest levels were found in wheat bran (1160 µg kg^?1), rye kernels (288 µg kg^?1) and oat flakes (55 µg kg^?1). The type B trichothecene nivalenol was detected in 67% of the wheat samples, in 3% of the rye samples and in 24% of the oat samples with highest levels in wheat bran (96 µg kg^?1), rye kernels (1.8 µg kg^?1) and in oat flakes (17 µg kg^?1), respectively. Levels of other type A and B trichothecenes played a minor role, although the rates of contamination were often high. Neither macrocyclic type D trichothecenes (satratoxin G and H, verrucarin A, roridin A) nor diacetylverrucarol and verrucarol (type A trichothecenes), were detected in any of the samples.     

A comparative study of high resolution cone beam X-ray tomography and synchrotron tomography applied to Fe- and Al-alloys

X-ray computed tomography (XCT) has become a very important method for non-destructive 3D-characterization and evaluation of materials. Due to measurement speed and quality, XCT systems with cone beam geometry and matrix detectors have gained general acceptance. Continuous improvements in the quality and performance of X-ray tubes and XCT devices have led to cone beam CT systems that can now achieve spatial resolutions down to 1 μm and even below. However, the polychromatic nature of the source, limited photon flux and cone beam artefacts mean that there are limits to the quality of the CT-data achievable; these limits are particularly pronounced with materials of higher density like metals. Synchrotron radiation offers significant advantages by its monochromatic and parallel beam of high brilliance. These advantages usually cause fewer artefacts, improved contrast and resolution.Tomography data of a steel sample and of two multi-phase Al-samples (AlSi12Ni1, AlMg5Si7) are recorded by advanced cone beam XCT-systems with a μ-focus (μXCT) and a sub-μm (nano-focus, sub-μXCT) X-ray source with voxel dimensions between 0.4 and 3.5 μm and are compared with synchrotron computed tomography (sXCT) with 0.3 μm/voxel. CT data features like beam hardening and ring artefacts, detection of details, sharpness, contrast, signal-to-noise ratio and the grey value histogram are systematically compared. In all cases μXCT displayed the lowest performance. Sub-μXCT gives excellent results in the detection of details, spatial and contrast resolution, which are comparable to synchrotron-XCT recordings. The signal-to-noise ratio is usually significantly lower for sub-μXCT compared with the two other methods. With regard to measurement costs “for industrial users”, scanning volume, accessibility and user-friendliness sub-μXCT has significant advantages in comparison to synchrotron-XCT.