Publisher Correction: Characterization of nitrogen doped graphene bilayers synthesized by fast, low temperature microwave plasma-enhanced chemical vapour deposition.

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Characterization of nitrogen doped grapheme bilayers synthesized by fast, low temperature microwave plasma-enhanced chemical vapour deposition.

New techniques to manipulate the electronic properties of few layer 2D materials, unveiling new physical phenomena as well as possibilities for new device applications have brought renewed interest to these systems. Therefore, the quest for reproducible methods for the large scale synthesis, as well as the manipulation, characterization and deeper understanding of these structures is a very active field of research. We here report the production of nitrogen doped bilayer graphene in a fast single step (2.5 minutes), at reduced temperatures (760 °C) using microwave plasma-enhanced chemical vapor deposition (MW-PECVD). Raman spectroscopy confirmed that nitrogen-doped bilayer structures were produced by this method. XPS analysis showed that we achieved control of the concentration of nitrogen dopants incorporated into the final samples. We have performed state of the art parameter-free simulations to investigate the cause of an unexpected splitting of the XPS signal as the concentration of nitrogen defects increased. We show that this splitting is due to the formation of interlayer bonds mediated by nitrogen defects on the layers of the material. The occurrence of these bonds may result in very specific electronic and mechanical properties of the bilayer structures.

Cell growth on 3D microstructured surfaces.

Chinese Hamster Ovary (CHO) cell cultures were grown on surfaces lithographed with periodic 3D hexagonal microcavity array morphology. The range of microcavity size (inscribed circle diameter) was from 12 µm to 560 µm. CHO cells were grown also on flat surfaces. The characterization was performed with respect to cell growth density (number of nuclei per unit area) by fluorescence optical microscopy and evaluated by correlation function analysis. We found that optimum microcavity radius was 80 µm, concerning to the maximum cell growth density, being even greater than the growth density on a flat (unstructured) substrate of the same material. This finding can be important for optimization of biotechnological processes and devices.

CO2 Laser Glazing Treatment of a Veneering Porcelain: Effects on Porosity, Translucency, and Mechanical Properties.

This work tested CO2 laser as a glazing agent and investigated the effects of irradiation on the porosity, translucency, and mechanical properties of veneering porcelain. Sixty discs (diameter 3.5 × 2.0 mm) of veneering porcelain for Y-TZP frameworks (VM9, VITA Zahnfabrik) were sintered and had one of their faces mirror polished. The specimens were divided into six groups (n=10/group) according to surface treatment, as follows: no treatment-control; auto-glaze in furnace following manufacturer's instructions (G); and CO2 laser (45 or 50 W/cm(2)) applied for four or five minutes (L45/4, L45/5, L50/4, L50/5). Optical microscopy (Shimadzu, 100×) was conducted and the images were analyzed with Image J software for the determination of the following porosity parameters: area fraction, average size, and Feret diameter. The translucency parameter studied was masking ability, determined by color difference (ΔE) over black and white backgrounds (CM3370d, Konica Minolta). Microhardness and fracture toughness (indentation fracture) were measured with a Vickers indenter (HMV, Shimadzu). Contact atomic force microscopy (AFM) (50 × 50 µm(2), Nanoscope IIIA, Veeco) was performed at the center of one sample from each group, except in the case of L45/5. With regard to porosity and translucency parameters, auto-glazed and laser-irradiated specimens presented statistical similarity. The area fraction of the surface pores ranged between 2.4% and 5.4% for irradiated specimens. Group L50/5 presented higher microhardness when compared to the G group. The higher (1.1) and lower (0.8) values for fracture toughness (MPa.m(1/2)) were found in laser-irradiated groups (L50/4 and L45/4, respectively). AFM performed after laser treatment revealed changes in porcelain surface profile at a submicrometric scale, with the presence of elongated peaks and deep valleys.

Gold ion implantation into alumina using an "inverted ion source" configuration.

We describe an approach to ion implantation in which the plasma and its electronics are held at ground potential and the ion beam is injected into a space held at high negative potential, allowing considerable savings both economically and technologically. We used an "inverted ion implanter" of this kind to carry out implantation of gold into alumina, with Au ion energy 40 keV and dose (3-9) × 10(16) cm(-2). Resistivity was measured in situ as a function of dose and compared with predictions of a model based on percolation theory, in which electron transport in the composite is explained by conduction through a random resistor network formed by Au nanoparticles. Excellent agreement is found between the experimental results and the theory.

Performance of an inverted ion source.

Whereas energetic ion beams are conventionally produced by extracting ions (say, positive ions) from a plasma that is held at high (positive) potential, with ion energy determined by the potential drop through which the ions fall in the beam formation electrode system, in the device described here the plasma and its electronics are held at ground potential and the ion beam is formed and injected energetically into a space maintained at high (negative) potential. We refer to this configuration as an "inverted ion source." This approach allows considerable savings both technologically and economically, rendering feasible some ion beam applications, in particular small-scale ion implantation, that might otherwise not be possible for many researchers and laboratories. We have developed a device of this kind utilizing a metal vapor vacuum arc plasma source, and explored its operation and beam characteristics over a range of parameter variation. The downstream beam current has been measured as a function of extraction voltage (5-35 kV), arc current (50-230 A), metal ion species (Ti, Nb, Au), and extractor grid spacing and beamlet aperture size (3, 4, and 5 mm). The downstream ion beam current as measured by a magnetically-suppressed Faraday cup was up to as high as 600 mA, and with parametric variation quite similar to that found for the more conventional metal vapor vacuum arc ion source.

Environmental effects in Kelvin force microscopy of modified diamond surfaces.

We have explored the effects of atmospheric environment on Kelvin force microscopy (KFM) measurements of potential difference between different regions of test polycrystalline diamond surfaces. The diamond films were deposited by microwave plasma-assisted chemical vapor deposition, which naturally produces hydrogen terminations on the surface of the films formed. Selected regions were patterned by electron-beam lithography and chemical terminations of oxygen or fluorine were created by exposure to an oxygen or fluorine plasma source. For KFM imaging, the samples were mounted in a hood with a constant flow of helium gas. Successive images were taken over a 5-h period showing the effect of the environment on KFM imaging. We conclude that the helium flow removes water molecules adsorbed on the surface of the samples, resulting in differences in surface potential between adjacent regions. The degree of water removal is different for surfaces with different terminations. The results highlight the importance of taking into account the atmospheric environment when carrying out KFM analysis.

A high voltage pulse power supply for metal plasma immersion ion implantation and deposition.

We describe the design and implementation of a high voltage pulse power supply (pulser) that supports the operation of a repetitively pulsed filtered vacuum arc plasma deposition facility in plasma immersion ion implantation and deposition (Mepiiid) mode. Negative pulses (micropulses) of up to 20 kV in magnitude and 20 A peak current are provided in gated pulse packets (macropulses) over a broad range of possible pulse width and duty cycle. Application of the system consisting of filtered vacuum arc and high voltage pulser is demonstrated by forming diamond-like carbon (DLC) thin films with and without substrate bias provided by the pulser. Significantly enhanced film∕substrate adhesion is observed when the pulser is used to induce interface mixing between the DLC film and the underlying Si substrate.

Small plasma source for materials application.

We describe a small hollow-cathode plasma source suitable for small-scale materials synthesis and modification application. The supporting electrical system is minimal. The gaseous plasma source delivers a plasma ion current of up to about 1 mA. Here we outline the source construction and operation, and present some of its basic performance characteristics.

Atomic force microscope nanolithography of polymethylmethacrylate polymer.

We describe a nanolithography process for a polymethylmethacrylate (PMMA) surface using scanning contact atomic force microscopy. Parallel furrows were scribed with a pyramidal silicon tip using the same scan mechanism as used to image samples. The PMMA was first electron beam irradiated using a scanning electron microscope and developed. The topography formed is reproducible and predictable. Material from the region where the tip scribes is moved to nearby regions, and aligned, elongated PMMA fragments are seen to decorate the valleys between furrows.

Cavity generation in dental enamel using a copper-HyBrID laser.

Applications of Cu-HyBrID laser (copper laser with Hydrogen Bromide In Discharge) in Dentistry and AFM (atomic force microscopy) evaluations of dental tissues irradiated by laser are seldom reported in the literature. This work presents an AFM investigation of the cross-section of a cavity generated in human dental enamel by laser thermal evaporation using the Cu-HyBrID laser. The results exposed the structural and morphological differences between the fused and non-fused dental enamel, provide qualitative information about the susceptibility of these tissues to abrasive polishing, and revealed the extension of the thermal damage. Quantitative information concerning the wall thickness and the dimensions of the cross-section of non-fused enamel rod were also obtained.

Carbamazepine: a bioequivalence study and limited sampling modeling.

OBJECTIVES: To assess the bioequivalence of 2 formulations of carbamazepine and to develop and validate limited sampling strategy (LSS) models for estimating the area under the plasma concentration-time curve (AUC0-infinity) and the peak plasma concentration (Cmax) of carbamazepine. METHODS: Twenty-four (12 men, 12 women) healthy volunteers received single oral doses (400 mg) of carbamazepine, as reference and test conventional-release formulations, in a standard 2-sequence, 2-period crossover design. Bioequivalence assessment was based on the individual ratios of log-transformed values of AUC0-infinity and Cmax LSS modeling was developed in a training set of 12 randomly assigned volunteers and was validated on the other 12 subjects (validation set). RESULTS: Carbamazepine AUC0-infinity and Cmax can be accurately predicted (R2 = 0.89 - 0.95, precision = 2.6 - 7.2%) by single-point (72 h) and 2-point LSS models (6, 32 h), respectively. Bioequivalence assessments based on LSS-derived AUC0-infinity and Cmax provided results similar to those obtained using all the concentration-in-plasma data points, and indicated that the 2 formulations are bioequivalent. CONCLUSION: One-and 2-point LSS models provided accurate estimates of carbamazepine's AUC0-infinity and Cmax, and allowed correct assessment of bioequivalence between the formulations studied.

Effects of caffeine on locomotor activity of horses: determination of the no-effect threshold.

Caffeine is the legal stimulant consumed most extensively by the human world population and may be found eventually in the urine and/or blood of race horses. The fact that caffeine is in foods led us to determine the highest no-effect dose (HNED) of caffeine on the spontaneous locomotor activity of horses and then to quantify this substance in urine until it disappeared. We built two behavioural stalls equipped with juxtaposed photoelectric sensors that emit infrared beams that divide the stall into nine sectors in a 'tic-tac-toe' fashion. Each time a beam was interrupted by a leg of the horse, a pulse was generated; the pulses were counted at 5-min intervals and stored by a microcomputer. Environmental effects were minimized by installing exhaust fans producing white noise that obscured outside sounds. One-way observation windows prevented the animals from seeing outside. The sensors were turned on 45 min before drug administration (saline control or caffeine). The animals were observed for up to 8 h after i.v. administration of 2.0, 2.5, 3.0 or 5.0 mg caffeine kg(-1). The HNED of caffeine for stimulation of the spontaneous locomotor activity of horses was 2.0 mg kg(-1). The quantification of caffeine in urine and plasma samples was done by gradient HPLC with UV detection. The no-effect threshold should not be greater than 2.0 microg caffeine ml(-1) plasma or 5.0 microg caffeine ml(-1) urine.

Hydrocortisone concentrations in post-race urine from horses.

As hydrocortisone is an endogenous substance, it is first necessary to establish its normal concentrations so as to be able to control its use in racing animals. This study was designed to establish the hydrocortisone concentrations in post-race urine samples of horses racing in Brazil and also to evaluate the results in relation to the international threshold set for this drug. Urine samples were analysed by HPLC-UV. The results were evaluated according to the concentration range as well as sex and time of sample collection (afternoon or evening races). The results showed a high degree of variation in the concentrations of hydrocortisone in the urine (93 +/- 69 ng/ml). The maximum concentration observed was 646 ng/ml, although only a few horses (around 1%) showed levels within the range 500-650 ng/ml, 91% being in the range 0-150 ng/ml. The data suggested a normal distribution curve. Statistical analysis showed no significant influence of sex or time of sample collection.

Immunoaffinity chromatography in the detection of dexamethasone in equine urine.

Due to the widespread use of dexamethasone in racing horses, mostly in low doses by intra-articular administration for the treatment of inflammatory processes, a method is developed to detect this drug in horse urine samples using liquid-liquid extraction followed by immunoaffinity chromatography. Liquid chromatography with diode-array detection is used for the identification of the drug. The use of immunoaffinity columns enhances the selectivity of the analysis, and the results show that dexamethasone can be detected up to 28 h after intra-articular administration.

The use of ELISA tests and immunoaffinity chromatography combined with reversed-phase high-performance liquid chromatography for dexamethasone detection in equine urine.

Dexamethasone is a corticosteroid drug widely used in racehorses because of its anti-inflammatory effect. It is, therefore, frequently detected in antidoping tests. A method for the antidoping control of dexamethasone in equine urine using screening by ELISA and confirmation by immunoaffinity chromatography combined with reversed-phase high-performance liquid chromatography-diode array detection (HPLC-DAD) is described. The ELISA test is frequently used in antidoping tests for its sensitivity, relative speed, and low cost. The test showed linearity in the range of 4-500 ng/mL of urine, and the intra-assay and interassay imprecision were 9.4 and 9.7%, respectively. The confirmation method showed a limit of detection of 4 ng/mL for dexamethasone. The intra-assay and interassay imprecisions were 10.3 and 14.4%, respectively. The HPLC-DAD showed a limit of detection of 5 ng and linearity in the range of 25-500 ng of dexamethasone. The absolute method recovery was 56.4%. The proposed method detected dexamethasone up to 52 h after administration and proved to be adequate for the antidoping control.

Determination of synthetic estrogens in illegal veterinary formulations by HPTLC and HPLC.

To determine the actual amount of diethylstilbestrol, hexestrol, and dienestrol in formulations such as pellets and oily injections that are illegally available on the Brazilian market, a simple methanol extraction is used for the analysis of the pellets and an ether extraction with Sephadex columns (for clean-up) is used for the oily injections. High-performance thin-layer chromatography is used for identification (as a qualitative and semiquantitative method), and high-performance liquid chromatography is used for quantitation. The results of the analysis show that all the formulations are not in accordance with the information listed on their labels.

Determination of phenylbutazone and oxyphenbutazone in plasma and urine samples of horses by high-performance liquid chromatography and gas chromatography-mass spectrometry.

A method is described for the qualitative and quantitative determination of phenylbutazone and oxyphenbutazone in horse urine and plasma samples viewing antidoping control. A horse was administered intravenously with 3 g of phenylbutazone. For the qualitative determination, a screening by HPLC was performed after acidic extraction of the urine samples and the confirmation process was realized by GC-MS. Using the proposed method it was possible to detect phenylbutazone and oxyphenbutazone in urine for up to 48 and 120 h, respectively. For the quantitation of these drugs the plasma was deproteinized with acetonitrile and 20 microliters were injected directly into the HPLC system equipped with a UV detector and LiChrospher RP-18 column. The mobile phase used was 0.01 M acetic acid in methanol (45:55, v/v). The limit of detection was 0.5 microgram/ml for phenylbutazone and oxyphenbutazone and the limit of quantitation was 1.0 microgram/ml for both drugs. Using the proposed method it was possible to quantify phenylbutazone up to 30 h and oxyphenbutazone up to 39 h after administration.

Determination of succinonitrile in horse urine by gas chromatography-nitrogen-phosphorus detector and gas chromatography-mass spectrometry.

A chromatographic method was developed to detect and confirm the presence of succinonitrile (SDN) in horse urine samples, for antidoping control. The urine samples (5 ml) were extracted with diethyl ether and screened by gas chromatography-nitrogen-phosphorus detector and the confirmation of the drug's presence was accomplished by using gas chromatography-mass selective detection. The recovery of extraction was 78 and 81% for 1.0 and 2.0 micrograms ml-1 (relative standard deviation, < 10%), respectively. Urine samples collected after the administration of Energisan were positive for SDN (1-30 h) in all samples analysed.

Determination of xanthines by high-performance liquid chromatography and thin-layer chromatography in horse urine after ingestion of Guaraná powder.

The seeds of Guaraná are rich in xanthines and are used for the preparation of guaraná powder which is very commonly given to horses as a 'tonic' in Brazil. In this paper, the xanthine content of guaraná powder was determined, in addition to its clearance time in horses. Thin-layer chromatography was used as a screening procedure and high-performance liquid chromatography was performed to quantify the drugs in both the powder and urine samples. The guaraná powder was found to contain 2.16, 1.10 and 36.78 mg g-1 of theobromine (TB), theophylline (TP) and caffeine (CF), respectively, and in urine it was possible to detect TB and TP up to 13 d and CF up to 9 d after the administration of guaraná powder.