High-throughput synthesis and characterization of Mg1−xCaxO films as a lattice and valence-matched gate dielectric for ZnO based field effect transistors

Using composition-spread technique, we have grown metastable Mg_1−xCa_xO solid solution films on ZnO layers by pulsed laser deposition. All the films exhibited (1 1 1) oriented cubic phase. Despite a large miscibility gap, no phase separation took place at growth temperatures up to 700 °C, whereas an optimal growth temperature was found at 400 °C in terms of the crystallinity. The composition-spread films were characterized by X-ray diffraction mapping technique. Both lattice parameters and diffraction intensity increased with increasing the CaO composition. The present isovalent heterointerfaces realized the perfect lattice-matching by properly adjusting the CaO composition, leading to particular interest for ZnO based field effect transistors.     

Preparation of the SrFe12O19-based magnetic composites via boron oxide glass devitrification

Magnetic composites were obtained in the system SrO–Fe₂O₃–B₂O₃ by oxide glass heat treatment at 600–950 °C. Samples of the composites were investigated using XRD analysis, magnetic measurements, electron microcopy, and thermal analysis. It was shown that chemical composition of the precursor oxide glass and thermal treatment conditions influenced on the SrFe₁₂O₁₉ particles morphology and magnetic properties. The composites and powders were obtained containing hexaferrite as single domain platelet crystals or polycrystalline aggregates with a coercive force up to 6300 Oe in the former case and 4200 Oe in the latter case.     

Preparation and textural characterisation of activated carbon from vine shoots (Vitis vinifera) by H3PO4—Chemical activation

An abundant and low-cost agricultural waste as vine shoots (Vitis vinifera) (VS), which is generated by the annual pruning of vineyards, has been used as raw material in the preparation of powder activated carbon (AC) by the method of chemical activation with phosphoric acid. After size reduction, VS were impregnated for 2 h with 60 wt.% H₃PO₄ solution at room temperature, 50 and 85 °C. The three impregnated products were carbonised at 400 °C. The product impregnated at 50 °C was heated either first at 150-250 °C and then at 400 °C or simply at 350-550 °C in N₂ atmosphere. The time of isothermal treatment after each dynamic heating was 2 h. The carbons were texturally characterised by gas adsorption (N₂, −196 °C), mercury porosimetry, and density measurements. FT-IR spectroscopy was also applied. Better developments of surface area and microporosity are obtained when the impregnation of VS with the H₃PO₄ solution is effected at 50 °C and for the products heated isothermally at 200 and 450 °C. The mesopore volume is also usually higher for the products impregnated and heated at intermediate temperatures.     

Synthesis, characterization and optical properties of multipod ZnO whiskers

Multipod ZnO whiskers were synthesized successfully by two steps: pulsed laser deposition (PLD) and thermal evaporation process. First, a thin layer of Zn films were deposited on Si(1 1 1) substrates by PLD. Then the whiskers grew on Zn-coated Si(1 1 1) substrate by the simple thermal evaporation oxidation of the metallic zinc powder at 900 °C in the air without any catalysts or additives. The pre-deposited Zn films by PLD on the substrate can promote the growth of ZnO multipod whiskers effectively. The as-synthesized ZnO whiskers were characterized by using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). The results revealed that the whiskers are highly crystalline with the wurtzite hexagonal structure. Room temperature photoluminescence (PL) spectrum of the whiskers shows a UV emission peak at ∼393 nm and a broad green emission peak at ∼517 nm, which was assigned to the near band-edge emission and the deep-level emission, respectively.     

K-induced surface structural change of Si(1 1 1)-7 × 7 probed by second-harmonic generation

The growth of thin K films on Si(1 1 1)-7 × 7 has been investigated by selecting the input and output polarizations of second-harmonic generation (SHG) at room temperature (RT) and at an elevated temperature of 350 °C. The SH intensity at 350 °C showed a monotonic increase with K coverages up to a saturated level, where low energy electron diffraction (LEED) showed a 3 × 1 reconstructed structure. The additional deposition onto the K-saturated surface at 350 °C showed only a marginal change in the SH intensity. These variations are different from the multi-component variations up to 1 ML and orders of magnitude increase due to excitation of plasmons in the multilayers at RT. The variations of SHG during desorption of K at 350 °C showed a two-step decay with a marked shoulder which most likely corresponds to the saturation K coverage of the Si(1 1 1)-3 × 1-K surface. The dominant tensor elements contributing to SHG are also identified for each surface.     

One convenient synthesis route to boron nitride nanotube

We describe one convenient synthesis route to boron nitride (BN) nanotube by the reaction of boron powder, iron oxide, and ammonium chloride at 600 °C for 12 h. Characterized by XRD, FTIR, XPS, TEM and SAED, the composition and morphology of the products are confirmed. The possible reaction mechanism is also discussed.     

Removal of chloridazon by natural and ammonium kerolite samples

The adsorption of chloridazon (5-amino-4-chloro-2-phenylpyridazin-3(2H)-one) on natural and ammonium kerolite samples from aqueous solution at 10, 25 and 40 °C has been studied by using batch experiments. The experimental data points were fitted to the Langmuir equation in order to calculate the adsorption capacities (X_m) of the samples; two straight lines were obtained, which indicates that the adsorption process takes place in two different stages. Values for X_m1 (first stage) ranged from 1.1 × 10⁻² mol kg⁻¹ for natural kerolite at 40 °C up to 5.1 × 10⁻² mol kg⁻¹ for ammonium kerolite at 10 °C and the values for X_m2 (second stage) ranged from 9.1 × 10⁻² mol kg⁻¹ for natural kerolite at 40 °C up to 14 × 10⁻² mol kg⁻¹ for natural kerolite at 10 °C. The adsorption experiments showed on the one hand, that the ammonium kerolite is more effective than natural kerolite to adsorb chloridazon in the range of temperature studied and on the other hand, that the lower temperature, the more effective the adsorption of chloridazon on the adsorbents studied.     

Preparation of activated carbons from cherry stones by activation with potassium hydroxide

Using cherry stones, the preparation of activated carbon has been undertaken in the present study by chemical activation with potassium hydroxide. A series of KOH-activated products was prepared by varying the carbonisation temperature in the 400-900 °C range. Such products were characterised texturally by gas adsorption (N₂, −196 °C), mercury porosimetry, and helium and mercury density measurements. FT-IR spectroscopy was also applied. The carbons prepared as a rule are microporous and macroporous solids. The degree of development of surface area and porosity increases with increasing carbonisation temperature. For the carbon heated at 900 °C the specific surface area (BET) is 1624 m² g⁻¹, the micropore volume is 0.67 cm³ g⁻¹, the mesopore volume is 0.28 cm³ g⁻¹, and the macropore volume is 1.84 cm³ g⁻¹.     

AFM investigation on surface evolution of amorphous carbon during ion-beam-assisted deposition

Hydrogen-free amorphous carbons (a-C) have been prepared on mirror-polished Si(1 1 1) wafers through thermally evaporated C₆₀ with simultaneous bombardments of Ne⁺ ions. The time evolution of film surfaces has been characterized by atomic force microscopy (AFM) at two temperatures of 400 and 700 °C, respectively. Based on the topography images and the root-mean-square (rms) roughness analysis, it is found that the a-C surfaces present roughening growth at the initial stage. With increasing growth time, the cooperative nucleation of the islands and pits appears on the surfaces, suggesting three-dimensional growth, and then they continue to evolve to irregular mounds at 400 °C, and elongated mounds at 700 °C. At the steady growth stage, these surfaces further develop to the structures of bamboo joints and ripples corresponding to these two temperatures, respectively. It is believed that besides ion sputtering effect, the chemical bonding configurations in the amorphous carbon films should be taken into considerations for elucidating the surface evolutions.     

Study of temperature dependence and angular distribution of poly(9,9-dioctylfluorene) polymer films deposited by matrix-assisted pulsed laser evaporation (MAPLE)

Poly(9,9-dioctylfluorene) (PFO) polymer films were deposited by matrix-assisted pulsed laser evaporation (MAPLE) technique. The polymer was diluted (0.5 wt%) in tetrahydrofuran and, once cooled to liquid nitrogen temperature, it was irradiated with a KrF excimer laser. 10,000 laser pulses were used to deposit PFO films on 〈1 0 0〉 Si substrates at different temperatures (−16, 30, 50 and 70 °C). One PFO film was deposited with 16,000 laser pulses at a substrate temperature of 50 °C. The morphology, optical and structural properties of the films were investigated by SEM, AFM, PL and FTIR spectroscopy. SEM inspection showed different characteristic features on the film surface, like deflated balloons, droplets and entangled polymer filaments. The roughness of the films was, at least partially, controlled by substrate heating, which however had the effect to reduce the deposition rate. The increase of the laser pulse number modified the target composition and increased the surface roughness. The angular distribution of the material ejected from the target confirmed the forward ejection of the target material. PFO films presented negligible modification of the chemical structure respect to the bulk material.     

Characterizations of n-type ferromagnetic GaMnN thin film grown on GaN/Al2O3 (0 0 0 1) by metal-organic chemical vapor deposition

A high-quality ferromagnetic GaMnN (Mn=2.8 at%) film was deposited onto a GaN buffer/Al₂O₃(0 0 0 1) at 885 °C using the metal-organic chemical vapor deposition (MOCVD) process. The GaMnN film shows a highly c-axis-oriented hexagonal wurtzite structure, implying that Mn doping into GaN does not influence the crystallinity of the film. No Mn-related secondary phases were found in the GaMnN film by means of a high-flux X-ray diffraction analysis. The composition profiles of Ga, Mn, and N maintain nearly constant levels in depth profiles of the GaMnN film. The binding energy peak of the Mn 2p_3/2 orbital was observed at 642.3 eV corresponding to the Mn (III) oxidation state of MnN. The presence of metallic Mn clusters (binding energy: 640.9 eV) in the GaMnN film was excluded. A broad yellow emission around 2.2 eV as well as a relatively weak near-band-edge emission at 3.39 eV was observed in a Mn-doped GaN film, while the undoped GaN film only shows a near-band-edge emission at 3.37 eV. The Mn-doped GaN film showed n-type semiconducting characteristics; the electron carrier concentration was 1.2×10²¹/cm³ and the resistivity was 3.9×10⁻³ Ω cm. Ferromagnetic hysteresis loops were observed at 300 K with a magnetic field parallel and perpendicular to the ab plane. The zero-field-cooled and field-cooled curves at temperatures ranging from 10 to 350 K strongly indicate that the GaMnN film is ferromagnetic at least up to 350 K. A coercive field of 250 Oe and effective magnetic moment of 0.0003 μ_B/Mn were obtained. The n-type semiconducting behavior plays a role in inducing ferromagnetism in the GaMnN film, and the observed ferromagnetism is appropriately explained by a double exchange mechanism.     

Growth of GaAs “nano ice cream cones” by dual wavelength pulsed laser ablation

Harmonic generation crystals inherently offer the possibility of using multiple wavelengths of light in a single laser pulse. In the present experiment, the fundamental (1064 nm) and second harmonic (532 nm) wavelengths from an Nd:YAG laser are focused together on GaAs and GaSb targets for ablation. Incident energy densities up to about 45 J/cm² at 10 Hz with substrate temperatures between 25 and 600 °C for durations of about 60 s have been used in an ambient gas pressure of about 10⁻⁶ Torr. The ablated material was collected on electron-transparent amorphous carbon films for TEM analysis. Apart from a high density of isolated nanocrystals, the most common morphology observed consists of a crystalline GaAs cone-like structure in contact with a sphere of liquid Ga, resembling an “ice cream cone”, typically 50-100 nm in length. For all of the heterostuctures of this type, the liquid/solid/vacuum triple junction is found to correspond to the widest point on the cone. These heterostructures likely form by preferential evaporation of As from molten GaAs drops ablated from the target. The resulting morphology minimizes the interfacial and surface energies of the liquid Ga and solid GaAs.     

Enhanced diamond nucleation on copper substrates by graphite seeding and CO2 laser irradiation

Diamond nucleation on copper (Cu) substrates was investigated by graphite seeding and CO₂ laser irradiation at initial stages of the combustion-flame deposition. A graphite aerosol spray was used to generate a thin layer of graphite powders (less than 1 μm) on Cu substrates. The graphite-seeded Cu substrates were then heated by a continuous CO₂ laser to about 750 °C within 1 min. It was found that diamond nucleation density after this treatment was more than three times as much as that on the virgin Cu substrates. As a consequence, diamond films up to 4 μm were obtained in 5 min. The enhancement of diamond nucleation on the graphite-seeded Cu substrates was attributed to the formation of defects and edges during the etching of the seeding graphite layers by the OH radicals in the flame. The defects and edges served as nucleation sites for diamond formation. The function of the CO₂ laser was to rapidly heat the deposition areas to create a favorable temperature for diamond nucleation and growth.     

Nano-graphene structures deposited by N-IR pulsed laser ablation of graphite on Si

Thin nano-structured carbon films have been deposited in vacuum by pulsed laser ablation, from a rotating polycrystalline graphite target, on Si 〈1 0 0〉 substrates, kept at temperatures ranging from RT to 800 °C. The laser ablation was performed by a Nd:YAG laser, operating in the near IR (λ = 1064 nm).X-ray diffraction analysis, performed at grazing incidence angle, both in-plane (ip-gid) and out-of-plane (op-gid), has shown the growth of oriented nano-sized graphene particles, characterised by high inter-planar stacking distance (d_? ∼ 0.39 nm), compared to graphite. The film structure and texturing are strongly related both to laser wavelength and substrate temperature: the low energy associated to the IR laser radiation (1.17 eV) generates activated carbon species of large dimensions that, also at low T (∼400 °C), easy evolve toward more stable sp² aromatic bonds, in the plume direction. Increasing temperature the nano-structure formation increases, causing a further aggregation of aromatic planes, voids formation, and a related density (by X-ray reflectivity) drop to very low values. SEM and STM show for these samples a strongly increased macroscopic roughness. The whole process, mainly at higher temperatures, is characterised by a fast kinetic mode, far from equilibrium and without any structural or spatial rearrangement.     

Carbon dioxide-activated carbons from almond tree pruning: Preparation and characterization

Activated carbons were prepared from almond tree pruning by non-catalytic and catalytic gasification with carbon dioxide and their surface characteristics were investigated. In both series a two-stage activation procedure (pyrolysis at 800 °C in nitrogen atmosphere, followed by carbon dioxide activation) was used for the production of activated samples. In non-catalytic gasification, the effect of the temperature (650-800 °C for 1 h) and the reaction time (1-12 h at 650 °C) on the surface characteristics of the prepared samples was investigated. Carbons were characterized by means of nitrogen adsorption isotherms at 77 K. The textural parameters of the carbons present a linear relation with the conversion degree until a value of approximately 40%, when they come independent from both parameters studied. The highest surface area obtained for this series was 840 m² g⁻¹. In the catalytic gasification the effect of the addition of one catalyst (K and Co) and the gasification time (2-4 h) on the surface and porosity development of the carbons was also studied. At the same conditions, Co leads to higher conversion values than K but this last gives a better porosity development.     

Infrared luminescence from spark-processed silicon

The infrared (IR) photoluminescence (PL) emission of spark-processed silicon (sp-Si) was investigated. A broad and strong room temperature PL peak in the 945 nm (1.31 eV) spectral range was observed when sp-Si was excited with an argon laser. This peak is different from the PL commonly reported for anodically etched porous silicon and other silicon-based materials. The PL intensity increases substantially after annealing sp-Si between 350 and 500 °C in air after which it decreases again. The PL wavelength is observed to peak at 1010 nm by annealing sp-Si near 450 °C. It was further found that the most efficient PL occurs for a Si/O ratio of 0.3, for a small spark gap of about 1 mm, and for spark-processing times in the 15-60 min range.A model for the IR PL is proposed which mirrors that for visible PL. Specifically, it is proposed that the electrons which have been pumped by the laser from the ground state into a broad quasi-absorption band (or closely spaced absorption lines between 1.7 and 2.3 eV) revert back to lower IR levels at 1.31 eV by a non-radiative transition from where they revert radiatively to the ground state by emitting the observed 945 nm light.     

Backside etching of fused silica with Nd:YAG laser

The laser-induced backside etching of fused silica with gallium as highly absorbing backside absorber using pulsed infrared Nd:YAG laser radiation is demonstrated for the first time. The influence of the laser fluence, the pulse number, and the pulse length on the etch rate and the etched surface topography was studied. The comparable high threshold fluences of about 3 and 7 J/cm² for 18 and 73 ns pulses, respectively, are caused by the high reflectivity of the fused silica-gallium interface and the high thermal conductivity of gallium. For the 18 and 73 ns long pulses the etch rate rises almost linearly with the laser fluence and reaches a value of 350 and 300 nm/pulse at a laser fluence of about 12 and 28 J/cm², respectively. Incubation processes are almost absent because etching is already observed with the first laser pulse at all etch conditions and the etch rate is constant up to 30 pulses.The etched grooves are Gaussian-curved and show well-defined edges and a smooth bottom. The roughness measured by interference microscopy was 1.5 nm rms at an etch depth of 0.6 μm. The laser-induced backside etching with gallium is a promising approach for the industrial application of the backside etching technique with IR Nd:YAG laser.     

Comparative study of ethanol sensor based on gold nanoparticles: ZnO nanostructure and gold: ZnO nanostructure

Gold colloid:ZnO nanostructures were prepared from Zn powder by using thermal oxidation technique on alumina substrates, then it was impregnated by gold colloid for comparative study. The gold colloid is the solution prepared by chemical reduction technique; it appeared red color for gold nanoparticle solution and yellow color for gold solution. The heating temperature and sintering time of thermal oxidation were 700 °C and 24 h, respectively under oxygen atmosphere. The structural characteristics of gold colloid:ZnO nanostructures and pure ZnO nanostructures were studied using filed emission scanning electron microscope (FE-SEM). From FE-SEM images, the diameter and length of gold colloid:ZnO nanostructures and ZnO nanostructures were in the ranges of 100-500 nm and 2.0-7.0 μm, respectively. The ethanol sensing characteristics of gold colloid:ZnO nanostructures and ZnO nanostructures were observed from the resistance alteration under ethanol vapor atmosphere at concentrations of 50, 100, 200, 500, and 1000 ppm with the operating temperature of 260-360 °C. It was found that the sensitivity of sensor depends on the operating temperature and ethanol vapor concentrations. The sensitivity of gold colloid:ZnO nanostructures were improved with comparative pure ZnO nanostructures, while the optimum operating temperature was 300 °C. The mechanism analysis of sensor revealed that the oxygen species on the surface was O²⁻.     

Preparation and characterization of carbons for the retention of halogens in the condenser vacuum system of a thermonuclear plant

Activated carbons were prepared by air and carbon dioxide activation, from almond tree pruning, with the aim of obtaining carbons that reproduce the textural and mechanical properties of the carbons currently used in the filtering system of the condenser vacuum installation of a Thermonuclear Plant (CNA; Central Nuclear de Almaraz in Caceres, Spain), produced from coconut shell. The variables studied in non-catalytic gasification series with air were the temperature (215-270 °C) and the time (1-16 h) and the influence of the addition of one catalyst (Co) and the time (1-2 h) in catalytic gasification. In the case of activation with CO₂, the influence of the temperature (700-950 °C) and the time (1-8 h) was studied. The resulting carbons were characterized in terms of their BET surface, porosity, and pore size distribution. The N₂ adsorption isotherms at 77 K for both series showed a type I behaviour, typical of microporous materials. The isotherms showed that with both gasificant agents the temperature rise produced an increase in the carbon porosity. With regards to the activation time, a positive effect on the N₂ adsorbed volume on the carbons was observed. The best carbons of each series, as well as the CNA (carbon currently used in the CNA), were characterized by mercury porosimetry and iodine solution adsorption isotherms. The results obtained allowed to state that several of the carbons produced had characteristics similar to the carbon that is target of reproduction (which has S_BET of 741 m² g⁻¹, V_mi of 0.39 cm³ g⁻¹ and a iodine retention capacity of 429.3 mg g⁻¹): carbon C (gasification with CO₂ at 850 °C during 1 h), with S_BET of 523 m² g⁻¹, V_mi of 0.33 cm³ g⁻¹ and a iodine retention capacity of 402.5 mg g⁻¹, and carbon D (gasification with CO₂ at 900 °C during 1 h), whose S_BET is 672 m² g⁻¹, V_mi is 0.28 cm³ g⁻¹ and has a iodine retention capacity of 345.2 mg g⁻¹.     

Effect of growth temperature on the morphology and bonded states of SnO2 nanobaskets

The nanobaskets of SnO₂ were grown on in-house fabricated anodized aluminum oxide pores of 80 nm diameter using plasma enhanced chemical vapor deposition at an RF power of 60 W. Hydrated stannic chloride was used as a precursor and O₂ (20 sccm) as a reactant gas. The deposition was carried out from 350 to 500 °C at a pressure of 0.2 Torr for 15 min each. Deposition at 450 °C results in highly crystalline film with basket like (nanosized) structure. Further increase in the growth temperature (500 °C) results in the deterioration of the basket like structure and collapse of the alumina pores. The grown film is of tetragonal rutile structure grown along the [1 1 0] direction. The change in the film composition and bonded states with growth temperature was evident by the changes in the photoelectron peak intensities of the various constituents. In case of the film grown at 450 °C, Sn 3d_5/2 is found built up of Sn⁴⁺ and O-Sn⁴⁺ and the peaks corresponding to Sn²⁺ and O-Sn²⁺ were not detected.