Sur la fiabilité du pic 1s du carbone de contamination comme étalon interne d'énergie dans les spectres de photoélectrons

The hydrocarbon contamination of an AEI ES 100 spectrometer has been studied in order to determine the reliability of the C 1s line as a standard in X-ray photoelectron spectra of non conducting solids. With alumina samples, it is shown that the contamination layer of this non ultra-high vacuum spectrometer is a suitable standard of energy for the correction of the charging effect and that it gives relative measurements with an accuracy of ± 0.2 eV when the sample temperature is varied from ?180°C to 200dgC or the sample holder is biased between ?10 and 10 V. About 75 spectra were recorded with powdered alumina compressed into a copper grid and the standard deviations of the corrected kinetic energies of the Al 2p and O 1s photoelectrons are respectively 0.09 and 0.06 eV.No effects of the X-ray tube current and the irradiation time are detected. The charging effect increases with the sample temperature (+0.6 eV from ?180 to 200°C).     

Preparation of Cu2O nanowires by thermal oxidation-plasma reduction method

Facial synthesis of cuprous oxide (Cu₂O) nanowires by directly heating copper substrates is difficult; however, in this study, it was successfully done by thermal oxidation followed by a plasma reduction process. The preparation of CuO nanowires with an average diameter of 76.2?nm supported on the surface of copper substrate was conducted first in air at 500?°C for 3?hrs, and then the CuO nanowires were reduced into Cu₂O in 15?min using either radio frequency (RF) N₂ plasma or microwave (MW) N₂ plasma. The characteristics of CuO and Cu₂O nanowires were analyzed using XRD, FE-SEM, and TEM. The results showed that Cu₂O nanowires can be successfully reduced from CuO nanowires by a simple, promising, and fast nitrogen plasma process. Moreover, in RF plasma, narrower and longer Cu₂O nanowires can be produced as compared to MW plasma, because energetic N-containing species can reduce the nanowires at a relatively lower temperature.     

Facile synthesis of nanostructured CuO for low temperature NO2 sensing

Detection of environmental pollutant and health hazardous, nitrogen dioxide (NO₂) is reported using nanostructured CuO particulates (NPs). Powder X-ray diffraction and field emission scanning electron microscopy were used to probe crystalline phase and morphological details, respectively. Small crystallites of ∼10–12 nm and a strain of 4% were found in the leafy structure of CuO. Raman studies further supported the presence of nanosized CuO phase. This is the first instance of utilizing CuO NPs to detect 5 ppm of NO₂ even at a low operating temperature of 50 °C. The highest sensitivity for NO₂ was observed at 150 °C, for the first time, in CuO NPs. A low activation energy of 0.18 eV was found for sensing process. The CuO NPs sensor responded to NO₂ within a few seconds and recovered totally under a minute. The kinetics of the NO₂ gas adsorption on the CuO film surface was described following the Elovich model.     

Two ultrasonic applications for the synthesis of nanostructured copper oxide (II)

In this paper, we present two aspects of the ultrasonic for the synthesis of CuO (II) nanostructures. In the first ultrasound application, we made a copper tip for an ultrasonic probe transducer and used it for electrolysis and ultrasound irradiation processes. This method is named direct sonoelectrochemistry and compares with conventional electrochemistry. CuO (II) nanostructures are obtained after sintering for both direct sonoelectrochemistry method and conventional electrochemistry method. In the second application of ultrasound, the copper nanostructures were generated by the ultrasound ablation method, and then, the heating process was performed for oxidation. The formation of the copper and CuO (II) nanostructures is confirmed by the powder X-ray diffraction (XRD), the field emission electron microscopy (FESEM), and transmission electron microscopy (TEM). The results show that the direct sonoelectrochemistry method generates CuO (II) nanostructures 4.2 times more than conventional electrochemistry. The crystallite size in the electrochemistry methods and direct sonoelectrochemistry is 28.44 nm and 26.60 nm, respectively. The direct sonoelectrochemistry way is a very flexible method and parameters in electrochemical, ultrasound, and the relationship between them can play an important role in the process of synthesis of nanostructures. The crystallite size in the ultrasound ablation method is 21.13 nm and 25.23 nm for the copper and CuO (II) nanostructures. The most important advantages of this method are green, fast, and high purity of the produced nanostructures.     

Effect of carbon nanotube addition on the thermite reaction in the Al/CuO energetic nanocomposite

Abstract

In this work, the Al/CNT/CuO nano-thermite samples are prepared by ultrasonic mixing with variable CNT content. The morphology of nano-thermites analysed by electron microscopy revealed that the CNTs are dispersed and there are intimate contacts between fuels (Al and CNT) and oxidiser (CuO) constituents of the nano-thermite. Raman spectroscopy technique is used to analyse the structural integrity of the CNTs in the nano-thermite. The thermite reaction characteristics are evaluated by simultaneous thermogravimetric analysis/differential scanning calorimetry technique. The exothermic enthalpy of the Al/CNT/CuO nano-thermite samples increased with increasing CNT content. The effect of Al particle size and Al/Cu molar ratio variation on the thermite reaction enthalpy is also analysed. The ignition temperature of the thermite reaction is also lowered by 71 °C than that of Al/CuO nano-thermite. The activation energy for thermite reaction of Al/CNT/CuO nano-thermite is also lowered by 23% to that of pure Al/CuO. The residues of the nano-thermites after the thermite reaction at 1010 °C are collected and analysed by the X-ray diffraction.     

Influence of 120 MeV Si9+ ion irradiation on ZnTe semiconductor thin films

ABSTRACT

ZnTe (Zinc Telluride) is a potential semiconducting material for many optoelectronic devices like solar cells and back contact material for CdTe-based solar cells. In the present study, ZnTe thin films were prepared by thermal evaporation technique and then irradiated with 120?MeV Si⁹⁺ ions at different fluences. These films are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV–Visible spectroscopy techniques. XRD study confirms increased crystallinity and grain growth for post-irradiated ZnTe thin films for fluences, up to 1?×?10¹¹ ions cm^?2. However, the grain size and crystallinity decreased for higher fluence-exposed samples. SEM images confirm the observed structural properties. Modification of the surface morphology of the film due to the ion irradiation with different fluences is studied. Optical band gap of film is decreased from 2.31?eV (pristine) to 2.17?eV after irradiation of Si⁹⁺ ions.     

Track revelation and optical properties of pentaerythritol tetrakis (allyl carbonate) plastic for application as nuclear track detector: effects of gamma radiations

The etching conditions of an indigenously prepared thin film of pentaerythritol tetrakis(allyl carbonate) (PETAC) were standardised for the use as a nuclear track detector. The optimum etching times in 6?N NaOH at 70°C for the appearance of fission and alpha tracks recorded in this detector from a ²⁵²Cf solid source were found to be 30 min and 1.50?h, respectively. The experimentally determined values for the bulk and track-etch rates for this detector in 6?N NaOH at 70°C were found to be 1.7?±?0.1 and 88.4?±?10.7?µm/h, respectively. From these results, the important track etching properties such as the critical angle of etching, the sensitivity and the fission track registration efficiency were calculated and compared with the commercially available detectors. The activation energy value for bulk etching calculated by applying Arrhenius equation to the bulk etch rates of the detector determined at different etching temperatures was found to be 0.86?±?0.02?eV. This compares very well with the value of about 1.0?eV reported for most commonly used track detectors. The effects of gamma irradiation on this new detector in the dose range of 200–1000?kGy have also been studied using bulk etch rate technique. The activation energy values for bulk etching calculated from bulk etch rates measurements at different temperatures were found to decrease with the increase in gamma dose indicating scission of the detector due to gamma irradiation. The optical band gap of this detector was also determined using UV–visible spectrometry and the value was found to be 4.37?±?0.05?eV.     

Preparation of CuO nanoparticles by metal salt-base reaction in aqueous solution and their metallic bonding property

This article describes a method for preparing CuO nanoparticles in aqueous solution, and a demonstration of feasibility of metallic bonding with the use of the CuO particles. Colloid solution of CuO nanoparticles was prepared from Cu(NO₃)₂ aqueous solution (0.01 M) and NaOH aqueous solution (0.019 M) at 5–80 °C. Leaf-like aggregates with an average size of 567 nm composed of CuO nanoparticles were produced at 20 °C. The size of leaf-like aggregates decreased with increasing reaction temperature. Metallic copper discs could be bonded using the CuO nanoparticles under annealing at 400 °C and pressurizing at 1.2 MPa for 5 min in H₂ gas. A shear strength required for separating the bonded discs was 25.4 MPa for the CuO nanoparticles prepared at 20 °C, whose aggregates were the largest among the CuO particles examined. These results indicated that the formation of leaf-like aggregates of CuO nanoparticles led to efficient metallic bonding.     

Utilization of ultrasonic irradiation as a green and effective strategy to prepare poly(N-vinyl-2-pyrrolidone)/modified nano-copper (II) oxide nanocomposites

The present paper describes the result of investigations into preparation of novel nanocomposites (NCs) based on poly(N-vinyl-2-pyrrolidone) (PVP) as a biocompatible polymer and modified copper (II) oxide nanoparticles (NPs) as a nano-filler. To achieve optimum NCs properties, different ratios of modified copper (II) oxide NPs (3, 5, and 7 wt%) were used to fabricate PVP NCs and also the ultrasonic irradiation was utilized to perform these processes as a fast and effective method. Subsequently, the structure of the obtained nanohybrids was characterized by various techniques. The suitable incorporation between PVP matrix and modified CuO NPs can be seen from the FT-IR spectra. The obtained NCs indicated an efficient thermal improvement in comparison to the pristine polymer. Also, the uniform dispersion of modified CuO NPs in the PVP matrix was detected by FE-SEM and EDX. According to UV absorption spectra, it is clear that these NCs can be used in UV protecting applications.     

Air stable colloidal copper nanoparticles: Synthesis,characterization and their surface-enhanced Raman scattering properties

Air stable colloidal copper nanoparticles are synthesized by a simple chemical reduction method using octadecylsilane as a reducing agent and octadecylamine as a stabilizing agent in toluene without any inert gas. The formation of nanosized copper was confirmed by its characteristic surface plasmon absorption peaks in UV–visible spectra. The transmission electron microscopic (TEM) images show that the resulting copper nanoparticles are distributed uniformly with a narrow size distribution. The X-ray diffraction (XRD) demonstrated that the obtained copper nanoparticles are single crystalline nanoparticles. Fourier transform infra-red (FT-IR) spectroscopic data suggested that the silane Si–H is responsible for the reduction of copper ions. And also the resulting colloidal copper nanoparticles exhibit large surface-enhanced Raman scattering (SERS) signals.     

Influence of nitrogen implantation on thermoluminescence of synthetic quartz

Thermoluminescence (TL) of synthetic quartz exposed to beta irradiation following implantation with 60?keV N⁺ ions at fluences ranging between 1?×?10¹⁴ and 5?×?10¹⁵?ions/cm² is reported. The glow curve measured at 5°C/s typically consists of a prominent peak near 110°C, studied in this work, and minor glow peaks at around 130°C and 190°C. The TL intensity of the main peak increased both with implantation and with fluence of implantation. The dependence of the intensity on heating rate and fluence suggests that the implantation introduces new defects that may possibly act as recombination centres. The increase in TL intensity with the heating rate exhibited by implanted samples has been observed in other luminescence materials. This anti-quenching phenomenon has been described as a competition effect between multiple luminescence pathways in luminescence materials. Kinetic analysis of the main glow peak using the initial rise, various heating rate and glow curve deconvolution methods shows that the activation energy of the main peak is about 0.7?eV with no systematic change due to ion fluence.     

Synthesis and optical properties of nanocrystalline ZnO powders prepared by a direct thermal decomposition route

This paper reports the synthesis and optical properties of nanocrystalline ZnO powders with crystallite sizes of 32.5 (±1.4)–43.4 (±0.4) nm prepared by a direct thermal decomposition of zinc acetate at the temperatures of 400, 500, 600, and 700°C for 4 h. The structure of the prepared samples was studied by XRD and FTIR spectroscopy, confirming the formation of wurtzite structure. The morphology of the samples revealed by SEM was affected by the thermal decomposition temperature, causing the formations of both nanoparticles and nanorods with different size and shape in the samples. The synthesized powders exhibited the UV absorption below 400 nm (3.10 eV) with a well defined absorption peak at around 285 nm (4.35 eV). The estimated direct bandgaps were obtained to be 3.19, 3.16, 3.14, and 3.13 eV for the ZnO samples thermally decomposed at 400, 500, 600, and 700°C, respectively. All the samples exhibited room-temperature photoluminescence (PL) showing a strong UV emission band at ∼395 nm (3.14 eV), a weak blue band at ∼420 nm (2.95 eV), a blue–green band at ∼485 nm (2.56 eV), and a very weak green band at ∼529 nm (2.35 eV). The mechanisms responsible for photoluminescence of the samples are discussed.     

Modification induced by gamma irradiation in Bayfol CR 1-4 polycarbonate

Bayfol CR 1-4 polycarbonate is a class of polymeric solid state nuclear track detector which has many applications in various radiation detection fields. Samples from sheets of Bayfol have been irradiated with gamma doses ranging from 100 to 620 kGy. The structural modifications in the gamma-irradiated Bayfol samples have been studied as a function of dose, using different characterization techniques such as X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy, intrinsic viscosity and refractive index. The results indicate that the carbonyl group (C?O) degraded under irradiation up to 200 kGy. This degradation, reported by FTIR spectroscopy enhanced the degree of ordering in the degraded samples as revealed by the XRD technique. Above 200 and up to 620 kGy, cross-linking is achieved, leading to an increase in the intrinsic viscosity from 0.41 to 0.78 at 35°C, indicating an increase in the average molecular mass. On the other hand, the resultant effect of gamma irradiation on the thermal properties of Bayfol has been investigated using thermo-gravimetric analysis, results indicating that the gamma irradiation in the dose range 200–620 kGy led to a more compact structure of Bayfol polymer, which resulted in an improvement in its thermal stability with an increase in the activation energy of thermal decomposition due to cross-linking. In addition, the V–I characteristics of the polymer samples were performed, results indicated that at higher voltage, the conduction mechanism of Bayfol CR 1-4 was identified as the Poole–Frenkel type.     

Nanoplate-like CuO: hydrothermal synthesis,characterization, and electrochemical properties

Plate-like nanocrystalline CuO was synthesized via the hydrothermal process using copper nitrate trihydrate as inorganic precursor and 1,3-diaminoprapane which acts as a structure-directing template. The morphology, the structure, the crystallinity and the composition were studied through x-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). It was found that the hydrothermal reaction time had a marked effect on the morphology and particularly, on the particle size and the nature of the resulting products. The optical properties of the as-synthesized CuO nanoplatelets were studied by UV-visible diffuse reflectance spectra (DRS) and the values of the band were found to be 1.93 eV. Electrochemical measurements have revealed a reversible redox behavior with a doping/de-doping process corresponding to reversible cation intercalation/de-intercalation. This process is easier for the smaller sized Li⁺ cation compared to the larger Na⁺ cation and to the largest K⁺ cation.     

Annealing of γ-ray irradiated lithium compensated p-type silicon

Abstract

Annealing behavior of electrical properties and photoluminescence spectra both at 77 °K in electron-irradiated melt-grown n-GaAs were investigated. Defects electrically active in the Hall mobility and carrier removal anneal through two stages centered at 250° and 460 °K. From the temperature dependence of carrier concentration the existence of a defect level located near 0.15 eV below the conduction band is supposed. Several emission bands are resolved at 1.51, 1.47, 1.415, 1.305 and ～1.2 eV in photoluminescence experiments. Electron irradiation (1.5–2.0 MeV) causes a remarkable decrease in emission intensity of 1.51 and ～1.2 eV bands. Recovery of emission intensity occurs remarkably when samples are annealed to 520 °K which would correspond to the 460 °K annealing stage for carrier concentration and Hall mobility. The 250 °K annealing stage is not observed in photoluminescence experiments. The 1.415 eV peak appears clearly after irradiation and grows remarkably with the 520 °K annealing, especially in Si-doped samples, resulting in large reverse annealing. This band is tentatively speculated to be a complex of Si on As site with As vacancy. Moreover, in samples doped with Te a new emission band at 1.305 eV (9500 Å) is observed after 470°–620 °K annealing.     

Swift heavy ion provoked structural, optical and electrical properties in SnO2 thin films

SnO₂ thin films grown on glass substrates at 300 ^°C by reactive thermal evaporation and annealed at 600 ^°C were irradiated by 120 MeV Ag⁹⁺ ions. Though irradiation is known to induce lattice disorder and suppression of crystallinity, we observe grain growth at a certain fluence of irradiation. X-ray diffraction (XRD) revealed the crystalline nature of the films. The particle size estimated by Scherrer’s formula for the irradiated films was in the range 10–25 nm. The crystallite size increases with increase in fluence up to 1×10¹² ions?cm^?2, whereas after that the size starts decreasing. Atomic force microscope (AFM) results showed the surface modification of nanostructures for films irradiated with fluences of 1×10¹¹ ions?cm^?2 to 1×10¹³ ions?cm^?2. The UV–visible spectrum showed the band gap of the irradiated films in the range of 3.56 eV–3.95 eV. The resistivity decreases with fluence up to 5×10¹² ions?cm^?2 and starts increasing after that. Rutherford Backscattering (RBS) reveals the composition of the films and sputtering of ions due to irradiation at higher fluence.     

Ambient effect on optical absorption of Au nanoparticles dispersed within pores of mesoporous SiO2

A gold nanoparticles/monolithic mesoporous silica assembly was synthesized by ultrasonic irradiation of monolithic porous silica presoaked with precursor solution. Subsequent exposure to ambient air (ageing) and then drying at 120°C induce a new optical absorption peak around 470?nm (falling into the range from 460 to 475?nm) which is stable at room temperature, in addition to the normal surface plasmon resonance (SPR) of Au nanoparticles. Further drying results in the decline and disappearance of this peak, accompanied by increase of the normal SPR. If the sample, in which the new peak has disappeared due to long drying at 120°C, is exposed to the ambience once more, this peak will appear again after subsequent drying at 120°C, showing reversibility. Further experiments indicate that ambient ageing for a certain time plays a crucial role in the appearance of the new peak after subsequent drying at 120°C. Increased ageing time increases this peak. In addition, the ambient relative humidity and temperature during exposure are also important to the appearance of this peak. This peak may be associated with Au clusters with a size less than 1.5?nm. Based on the porous structure of the assembly and hydrophilicity of its pore wall, a nanodroplet formation and evaporation model is presented which can well explain all evolution behaviours of this peak. The model predicts the existence of the peak at 470?nm in the Au/silica assembly prepared by methods other than ultrasonic irradiation, which has also been confirmed by further experiments.     

Enlargement of the stability range and superconducting domain of the T/O type phase of the La2)CuO4-Nd2CuO4 system after treatment under oxygen pressure

Abstract

Two main solid solutions exist in the La(2)CuO(4)-Nd(Z)CuO(4) system. The structure of the first one is related to that of tetragonal K(2)NiF(4) and is labelled as T/O; copper ions are in sixfold coordination (elongated octahedron), The second one has an original structure, called T′, in which copper ions are in square planar coordination. When synthezised in air at 800°C, the upper limit of the T/O type solid solution is 0.55. By subsequent treatment under 40 MPa oxygen pressure between 920 and 94O°C, this limit is shifted up to ? 0.80, and an ultimate oxidation by electrochemistry induces a bulk superconductivity, as in the case of normaly prepared T/O phases (x ≥ 0.55). Data are given on the change in the unit cell parameters, deviation from oxygen stoichiometry and conduction properties consecutive to the oxidizing treatments.     

Anatase TiO<Subscript>2</Subscript> nanoparticles for lithium-ion batteries

Anatase TiO₂ nanoparticles were prepared by a simple sol-gel method at moderate temperature. X-ray powder diffraction (XRD) and Raman spectroscopy revealed the exclusive presence of anatase TiO₂ without impurities such as rutile or brookite TiO₂. Thermogravimetric analysis confirmed the formation of TiO₂ at about 400 °C. Particle size of about 20 nm observed by transmission electron microscopy matches well with the dimension of crystallites calculated from XRD. The electrochemical tests of the sol-gel-prepared anatase TiO₂ show promising results as electrode for lithium-ion batteries with a stable specific capacity of 174 mAh g^?1 after 30 cycles at C/10 rate. The results show that improvement of the electrochemical properties of TiO₂ to reach the performance required for use as an electrode for lithium-ion batteries requires not only nanosized porous particles but also a morphology that prevents the self-aggregation of the particles during cycling.