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Abstract In this study, we have employed infrared (IR) absorption spectroscopy, visible Raman spectroscopy, and x-ray absorption near edge structure (XANES) to quantify the hydrogen (H) content in hydrogenated amorphous carbon (aC: H)... more
Abstract In this study, we have employed infrared (IR) absorption spectroscopy, visible Raman spectroscopy, and x-ray absorption near edge structure (XANES) to quantify the hydrogen (H) content in hydrogenated amorphous carbon (aC: H) films. aC: H films with a hydrogen content varying from 29 to 47 at.% have been synthesized by electron cyclotron resonance chemical vapor deposition at low substrate temperatures (≪ 120 C) applying a wide range of bias voltage, V b,(-300 V≪ V b≪+ 100 V).
Poly (vinylidene fluoride) (PVDF) composites with different types of nanodiamond (ND) particles were produced by solvent casting. The variations of the morphological, structural, optical, thermal and electrical properties of the... more
Poly (vinylidene fluoride) (PVDF) composites with different types of nanodiamond (ND) particles were produced by solvent casting. The variations of the morphological, structural, optical, thermal and electrical properties of the composites were studied as a function of nanofiller type (without and with air oxidation treatment) and concentration (in the range 0.1–1 wt%). No noticeable differences were found in the polymer crystallization process, the processing conditions and the filler determining the morphology and structure of the polymer. Nevertheless, ND nanofillers were useful for the tailoring of the optical properties, and also slightly contributed to the thermodynamic stability of the samples. An increase in the dielectric constant (∼2) of the ND composites, while maintaining constant the dielectric losses, was observed, independently of the filler concentration. On the other hand, solvent casted porous composites crystallize mainly in the electroactive γ-phase of PVDF. Those composite membranes were evaluated with pre-osteoblast culture tests and these revealed that the inclusion of ND nanoparticles does not induce cytotoxicity on the samples. Taking advantage of the properties of the polymer for cell culture and with the potential of the ND filler for protein functionalization and drug delivery, it is concluded that NDs/PVDF composites are a suitable platform for biomedical applications.
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This is a pioneering study on the synthesis and application of composites based on micro- and nanodiamonds for the photocatalytic degradation of environmental water pollutants. Micro- and nanodiamond powders (with particle sizes of 1–3 μm... more
This is a pioneering study on the synthesis and application of composites based on micro- and nanodiamonds for the photocatalytic degradation of environmental water pollutants. Micro- and nanodiamond powders (with particle sizes of 1–3 μm and 2–10 nm, respectively) were combined with TiO2, by varying the carbon-phase content, and tested as composite photocatalysts for the degradation of diphenhydramine, which is a pharmaceutical water pollutant, under near-UV/Vis irradiation. These composites exhibited higher photocatalytic activity than the respective bare materials. In addition, composites prepared with pristine nanodiamonds were always more active than those prepared with microdiamonds of the same carbon content. A significant enhancement in the photocatalytic performance was observed on preparation of the composite with 15 wt % of nanodiamonds oxidised in air at 703 K; these oxidised nanodiamonds contained mainly carboxylic anhydrides, lactones, phenols and, to a lesser extent, carbonyl/quinone groups on their surface.
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ABSTRACT Nitriding behaviour of pure chromium in an NH3–H2 atmosphere is discussed. Chromium samples were nitrided for various times (1, 4, 24, 48, 72, 120 and 142 h) at 800 °C. The nitridation is accompanied by an increase in surface... more
ABSTRACT Nitriding behaviour of pure chromium in an NH3–H2 atmosphere is discussed. Chromium samples were nitrided for various times (1, 4, 24, 48, 72, 120 and 142 h) at 800 °C. The nitridation is accompanied by an increase in surface porosity, which leads to an enlarged surface brittleness. Vickers microhardness measurements along the direction of nitrogen diffusion show an overall increase in hardness as a result of the nitriding process resulting in a surface hardness as high as about 1200–1400 Vickers. X-ray diffraction studies reveal the formation of Cr2N, CrN and Cr(N) phases upon nitriding. Scanning electron microscopy and energy dispersive X-ray analysis (EDAX) show an increasing fraction of the CrN phase formed at the surface with increasing nitriding times. EDAX line profile analysis of the specimen nitrided for 120 h shows a three-layered structure. Though the surface layer and the second layer adjacent to it, both consist of a mixture of CrN and Cr2N phases, the fraction of CrN is much higher in the surface layer. Nitridation of Cr2N is suggested as the possible mechanism for CrN formation at the surface with increasing nitriding times, for the nitriding parameters chosen in the present study.
The analytical performance of the newly proposed laser-based photoacoustic spectroscopy (PAS) and of optothermal window (OW) method for quantification of total anthocyanin concentration (TAC) in five sour cherry varieties is compared to... more
The analytical performance of the newly proposed laser-based photoacoustic spectroscopy (PAS) and of optothermal window (OW) method for quantification of total anthocyanin concentration (TAC) in five sour cherry varieties is compared to that of the spectrophotometry (SP). High performance liquid chromatography (HPLC) was used to identify and quantify specific anthocyanins. Both, PAS and OW are direct methods that unlike SP
ABSTRACT We have obtained simultaneously nanocrystalline and {100} faceted large-grained polycrystalline diamond films not only on different substrates but also on the same substrate in only one deposition run using a novel approach for... more
ABSTRACT We have obtained simultaneously nanocrystalline and {100} faceted large-grained polycrystalline diamond films not only on different substrates but also on the same substrate in only one deposition run using a novel approach for substrate arrangement. Furthermore, interesting unusual morphologies and microstructures composed by non-faceted nanostructures and terminated with large smooth {100} facet-like belt are found near the edges of the top square sample. The morphology variation is likely caused by the so called edge effect, where a strong variation in temperature is also present. We have modelled the temperature distribution on the substrates by computer simulations using the finite element method. The novel feature, namely the coexistence of oval non-faceted nanocrystalline diamond grains and large smooth {100} facet-like belt in one diamond grain, is in the transition from {100} faceted polycrystalline diamond to cauliflower-like nanocrystalline diamond. The formation mechanism is discussed based on the temperature analysis and other simulation results described in the literature. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)
... 1, each corner of sample PD1 has a large spot, which is actually a very big multi-twinned crystal of mm range size. As an example, Fig. 2b shows the much bigger multi-twinned crystal grown in the left corner as compared to the... more
... 1, each corner of sample PD1 has a large spot, which is actually a very big multi-twinned crystal of mm range size. As an example, Fig. 2b shows the much bigger multi-twinned crystal grown in the left corner as compared to the relatively smaller crystals grown along the edges. ...
ABSTRACT In this study, the use of thin Si interlayers (35–150 nm) for promoting diamond deposition onto steel is investigated. The diamond films are deposited by hot filament CVD onto AISI type 316 stainless and high-speed steels. Single... more
ABSTRACT In this study, the use of thin Si interlayers (35–150 nm) for promoting diamond deposition onto steel is investigated. The diamond films are deposited by hot filament CVD onto AISI type 316 stainless and high-speed steels. Single stage deposition at substrate temperatures ranging from as low as 475 to 750 °C is found to result only in non-continuous films with low number densities of diamond crystallites. A composite film of diamond and carbides is formed at intermediate temperatures of about 650 °C. It is believed that the formation of iron silicide phases at the exposed steel substrate surfaces leads to diffusion barriers for free iron from the steel matrix, so that graphitic soot formation is significantly avoided.Utilizing a two-stage deposition process, the density and uniformity of the deposited diamond films areincreased and a nearly continuous cauliflower shaped diamond film is obtained. Micro-Raman spectros-copy, scanning electron microscopy and X-ray diffraction techniques are employed to study the phases, morphology, composition, quality and residual stresses of the grown diamond layers.
Both ex situ and in situ atomic force microscopy have been applied to study the {111} and {100} surfaces of tabular silver bromide crystals grown from dimethyl sulphoxide–water solutions. This resulted in observations of monosteps,... more
Both ex situ and in situ atomic force microscopy have been applied to study the {111} and {100} surfaces of tabular silver bromide crystals grown from dimethyl sulphoxide–water solutions. This resulted in observations of monosteps, macrosteps, etch pits, pinning of steps and nucleated crystals showing twin planes. These examinations indicate that the growth and dissolution of both the {100} and
In this study the morphology and growth mechanism of AgX (X=Cl, Br) needle crystals will be revealed. The silver halide needles are grown by two different techniques. AgBr needles are grown with an extractive crystallization in a... more
In this study the morphology and growth mechanism of AgX (X=Cl, Br) needle crystals will be revealed. The silver halide needles are grown by two different techniques. AgBr needles are grown with an extractive crystallization in a dimethylsulfoxide–water mixture and AgCl needles are grown from the vapor phase. All needles contain nonparallel twin planes. The morphology of the AgBr needles
ABSTRACT By an extensive investigation of the principal growth parameters on the deposition process, we realized the epitaxial growth of crystalline wurtzite GaN thin films on single crystal (001) diamond substrates by metal organic... more
ABSTRACT By an extensive investigation of the principal growth parameters on the deposition process, we realized the epitaxial growth of crystalline wurtzite GaN thin films on single crystal (001) diamond substrates by metal organic chemical vapor deposition. From the influence of pressure, V/III ratio, and temperature, it was deduced that the growth process is determined by the mass-transport of gallium precursor material toward the substrate. The highest temperature yielded an improved epitaxial relationship between grown layer and substrate. X ray diffraction (XRD) pole figure analysis established the presence of two domains of epitaxial layers, namely (0001) 〈 10 0〉 GaN∥ (001)[110] diamond and (0001) 〈 10 0〉 GaN∥ (001) [10] diamond, which are 90∘ rotated with respect to each other. The presence of these domains is explained by the occurrence of areas of (2×1) and (1×2) surface reconstruction of the diamond substrate. When applying highly misoriented diamond substrates toward the [110] diamond direction, one of the growth domains is suppressed and highly epitaxial GaN on (001) diamond is realized.
The in situ electrochemical deposition of nanostructured MoSx (x=1.5–1.7) based thin films on various substrates from aqueous solutions is reported. The as-deposited amorphous films transform on annealing into crystalline ones as revealed... more
The in situ electrochemical deposition of nanostructured MoSx (x=1.5–1.7) based thin films on various substrates from aqueous solutions is reported. The as-deposited amorphous films transform on annealing into crystalline ones as revealed by a stepwise high temperature X-ray diffraction (XRD). Both Raman spectroscopy and XRD crystal structure analyses confirmed the formation of inorganic fullerene-MoSx nanoparticles (IF-MoSx). The as-deposited thin films
We investigated the mechanical and tribological properties of hydrogenated amorphous carbon (aC: H) films on silicon substrates by nanoindentation, ball-on-disc tribotesting and scratch testing. The aC: H films were deposited from an... more
We investigated the mechanical and tribological properties of hydrogenated amorphous carbon (aC: H) films on silicon substrates by nanoindentation, ball-on-disc tribotesting and scratch testing. The aC: H films were deposited from an argon/methane gas mixture by bias-enhanced electron cyclotron resonance chemical vapour deposition (ECR-CVD). We found that substrate biasing directly influences the hardness, friction and wear resistance of the aC: H films. An abrupt change in these properties is observed at a substrate bias of about− ...
This paper reports on hot filament CVD diamond deposition onto steel using arc-plated chromium nitride (CrN) as the interlayer. Direct deposition of diamond onto steel leads to the formation of a non-adhering layer of graphitic soot... more
This paper reports on hot filament CVD diamond deposition onto steel using arc-plated chromium nitride (CrN) as the interlayer. Direct deposition of diamond onto steel leads to the formation of a non-adhering layer of graphitic soot covered by poor-quality diamond. However, if ...
The influence of nitrogen addition on the properties of oxyacetylene flame-deposited diamond has been studied by means of X-ray diffraction (XRD), micro-Raman spectroscopy and cathodoluminescence spectroscopy (CL). A morphological... more
The influence of nitrogen addition on the properties of oxyacetylene flame-deposited diamond has been studied by means of X-ray diffraction (XRD), micro-Raman spectroscopy and cathodoluminescence spectroscopy (CL). A morphological transition reported in earlier work was found to have a major influence on the diamond properties. XRD indicated the presence of a molybdenum carbide layer in between the diamond film and
Abstract In the present work, aC: H films have been grown from argon/methane gas mixtures by Electron Cyclotron Resonance Chemical Vapour Deposition (ECRCVD). The effect of the application of a dc bias voltage to the silicon substrate... more
Abstract In the present work, aC: H films have been grown from argon/methane gas mixtures by Electron Cyclotron Resonance Chemical Vapour Deposition (ECRCVD). The effect of the application of a dc bias voltage to the silicon substrate material on the structural, morphological and mechanical properties of the films has been explored by multiple analysis techniques such as IR and micro-Raman spectroscopy, AFM, nano-indentation and pin-ondisk wear testing. In general, within the range of–300 V to+ 100 V applied substrate ...
Gold (1 wt.%) was loaded on several types of carbon materials (activated carbon, polymer based carbon xerogels, multi-walled carbon nanotubes, nanodiamonds, microdiamonds, graphite and silicon carbide) using two different methods (sol... more
Gold (1 wt.%) was loaded on several types of carbon materials (activated carbon, polymer based carbon xerogels, multi-walled carbon nanotubes, nanodiamonds, microdiamonds, graphite and silicon carbide) using two different methods (sol immobilisation and double impregnation). Samples were characterised by N2 adsorption at −196 °C, temperature programmed desorption, high-resolution transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray spectrometry, high-angle annular dark-field imaging (Z-contrast), X-ray photoelectron spectroscopy and atomic absorption spectroscopy. The obtained Au/carbon materials were used as catalysts for the oxidation of cyclohexane to cyclohexanol and cyclohexanone, with aqueous H2O2, under mild conditions. The most active catalyst was prepared by supporting gold nanoparticles on carbon nanotubes by the sol method, achieving an overall turnover number of ca. 171 and an overall yield of 3.6% after 6 h reaction time. These values are comparable to the industrial process (that uses Co catalysts and high temperature), but were obtained at ambient temperature with considerable low loads of catalyst (Au catalyst to substrate molar ratio always lower than 1 × 10−3), which is of relevance for establishing a greener catalytic process for cyclohexane oxidation. Moreover, a very high selectivity towards the formation of cyclohexanol and cyclohexanone was achieved, since no traces of by-products were detected. The promoting effect of pyrazine carboxylic acid was observed and an optimum peroxide-to-catalyst molar ratio was found to be 2 × 104. Further increase of the oxidant amount results in decreased yield due to overoxidation reactions at higher H2O2 amounts. Catalyst recycling was tested up to six consecutive cycles for the most active catalytic system (gold deposited on carbon nanotubes by sol immobilisation), and it was found that the catalyst maintains almost the original level of activity after several reaction cycles (there was only a 6% drop in activity after the sixth cycle) with a rather high selectivity to cyclohexanol and cyclohexanone and with no catalyst leaching. The differences in activity for the other samples can be explained in terms of gold nanoparticle size and the textural properties of the carbon support.
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Poly(vinylidene fluoride) (PVDF) composites with different carbonaceous nanofillers, prepared by solution casting, were studied their chemical, mechanical, electrical and electro-mechanical properties evaluated. Few-layer graphene (FLG)... more
Poly(vinylidene fluoride) (PVDF) composites with different carbonaceous nanofillers, prepared by solution casting, were studied their chemical, mechanical, electrical and electro-mechanical properties evaluated. Few-layer graphene (FLG) nanoplatelets (G-NPL), graphene oxide (GO) and reduced graphene oxide (rGO) and single-walled carbon nanohorns (SWCNH)) were found to have a strong influence in the overall properties of the composites prepared with up to 5 wt% nanofiller contents. The mechanical strain of carbonaceous nanofillers/PVDF composites decreases from 15% to near 5% of maximum strain. The electrical percolation threshold depends on the nanofiller type, being below 1 wt% for rGO and near 2 wt% for the remaining nanofillers. The electrical conductivity shows a maximum increase of nine orders of magnitude, from s z 5 Â 10 À11 S/m of pure PVDF to s z 1 Â 10 À2 S/m for rGO/PVDF composites with 5 wt% nanofillers. The conduction mechanism being related to hopping between the carbonaceous nanofillers for concentrations higher than the percolation threshold. Furthermore, the composites show electro-mechanical properties, except for G-NPL materials, with rGO/PVDF composites with 5 wt% nanofiller content showing higher Gauge factor (GF) values, reaching GFz 11 for deformations between 0.5 and 2 mm in 4-point bending experiments. These results demonstrate the suitability of the composites for strain sensing applications.