Coating and spark plasma sintering of nano-sized TiN on Y-α-sialon

TiN coating on Y-α-sialon was accomplished by depositing TiO₂ on their particle surfaces through controlled hydrolysis of TiCl₄ and Ti(O-i-C₃H₇)₄ and subsequent nitridation with NH₃ gas at 1000 °C. TiN particles covering Y-α-sialon were about 20 nm in size. Spark plasma sintering (SPS) of TiN/Y-α-sialon particles produced composite ceramics with continuous TiN networks at 1400 °C, but with TiN grains isolated in elongated β-sialon grains at 1600 °C. The relative density and Vickers hardness of TiN/sialon ceramics SPSed at 1400–1600 °C containing 25 vol.% TiN were measured. The electrical resistivity was in a wide range of 10⁻⁴ to 10⁰ Ω cm for the ceramics sintered at 1400 °C, but lowered to the order of magnitude of 10⁻¹ and 10⁵ Ω cm at higher temperatures ≥1500 °C. It was found that the complete transition to β-sialon increased the resistivity to 10³ to 10⁵ Ω cm, due to breaking up continuous TiN layers by elongated β-sialon grains.     

Influence of Ar/O2 ratio on the properties of transparent conductive ZnO:Ga films prepared by DC reactive magnetron sputtering

Ga-doped zinc oxide (ZnO:Ga) transparent conductive films with highly (002)-preferred orientation were deposited on glass substrates by DC reactive magnetron sputtering method in Ar + O₂ ambience with different Ar/O₂ ratios. The structural, electrical, and optical properties were investigated by X-ray diffraction, Hall measurement, and optical transmission spectroscopy. The resistivity and optical transmittance of the ZnO:Ga thin films are of the order of 10^− 4 Ω cm and over 85%, respectively. The lowest electrical resistivity of the film is found to be about 3.58 × 10^− 4 Ω cm. The influences of Ar/O₂ gas ratios on the resistivity, Hall mobility, and carrier concentration were analyzed.     

Performances of a-Si:H films produced by hot wire plasma assisted technique

This work reports on the performances of undoped and doped amorphous/nanocrystalline silicon films grown by hot wire plasma assisted technique. The structure (including the presence of several nanoparticles with sizes ranging from 5 nm to 50 nm), composition (oxygen and hydrogen content) and transport properties of the films are highly dependent on the temperature of the filament and on the hydrogen dilution. The undoped films grown under low r.f. power (≈4 mWcm⁻²) and filament temperatures around 1850 K present dark conductivities below 10⁻¹⁰ Scm⁻¹, optical gaps of about 1.6 eV and photosensitivities above 10⁵, (under AM1.5 light intensities), with almost no traces of oxygen content. For the n- and the p-doped silicon films also fabricated under the same conditions the conductivities obtained are of about 10⁻² Scm⁻¹ and 10⁻⁵ Scm⁻¹, respectively.     

Characteristics of Al-doped c-axis orientation ZnO thin films prepared by the sol–gel method

Transparent conducting ZnO thin films doped with Al have been prepared by sol–gel method, which were characterized by X-ray diffraction, atomic force microscopy and ultra-violet spectrometer. The films showed a hexagonal wurtzite structure and high preferential c-axis orientation. The optical transmittance spectra of the films showed the transmittance higher than 85% within the visible wavelength region. A minimum resistivity of 6.2 × 10⁻⁴ Ω cm was obtained for the film doped with 1.5 mol.% Al, preheated at 300 °C for 15 min and post-heated at 530 °C for 1 h.     

Tungsten-doped tin oxide thin films prepared by pulsed plasma deposition

Transparent conductive oxide tungsten-doped tin oxide thin films were deposited on glass substrates from ceramic targets by the pulsed plasma deposition method. The structural, electrical and optical properties have been investigated as functions of tungsten doping content and oxygen partial pressure. The lowest resistivity of 2.1 × 10^? 3 Ω?cm was reproducibly obtained, with carrier mobility of 30 cm²V^? 1s^? 1 and carrier concentration of 9.6 × 10¹⁹ cm^? 3 at the oxygen partial pressure of 1.8 Pa. The average optical transmission was in excess of 80% in the visible region from 400 to 700 nm, with the optical band gap ranging from 3.91 to 4.02 eV.     

Comparative study of NiFe2−xAlxO4 ferrite nanoparticles synthesized by chemical co-precipitation and sol–gel combustion techniques

A series of aluminum substituted Ni-ferrite nanoparticles have been synthesized by chemical co-precipitation and sol–gel techniques. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscope (AFM), Fourier transform infrared spectroscopy (FTIR), DC electrical resistivity and dielectric properties. Analysis of the X-ray diffraction pattern of all the samples confirmed the formation of spinel structure. The crystallite sizes remain within the range 25–41 ± 3 nm. FTIR measurements show two fundamental absorption bands, assigned to the vibration of tetrahedral and octahedral sites. DC electrical resistivity increases from 6.60 × 10⁷ to 6.9 × 10¹⁰ Ω cm as the Al³⁺ concentration increases from 0.00 to 0.50. The dielectric constant and loss tangent decreases with increasing Al³⁺ concentration from 22 to 14, 0.354 to 0.27 respectively at 5 MHz for all the samples. Impedance measurements as a function of frequency (1 kHz–5 MHz) at room temperature further helped in analyzing the electrical properties of the prepared samples.     

Synthesis and characterization of Co/SiO2 as catalyst catalyze hydrogen generation

Novel composites of porous SiO₂-LP and SiO₂-HP supports are synthesized by the silica–polyethylene glycol monooleyl ether surfactant self-assembly method to obtain a large surface area. Cobalt is immobilized in the supports by incipient wetness impregnation. A stable and active Co/SiO₂ catalyst is examined using FE-SEM, BET and XRD. Further, the catalyst is tested for catalytic hydrolysis of alkaline sodium borohydride (NaBH₄) solution: the rate of hydrogen generation is found to increase with increasing cobalt loading of the Co/SiO₂ catalyst. The hydrogen generation rates increase dramatically when the temperature is increased from 17 to 40 °C. The highest hydrogen generation rates of Co/SiO₂ catalyst are obtained at 2513 mL min^? 1 g^? 1 in 20 mL of 5 wt.% NaBH₄ solution containing 5 wt.% NaOH at 40 °C.     

Carbon fiber polymer–matrix structural composites exhibiting greatly enhanced through-thickness thermoelectric figure of merit

The through-thickness thermoelectric behavior of continuous carbon fiber epoxy-matrix composites is greatly improved by adding tellurium particles (13 vol.%), bismuth telluride particles (2 vol.%) and carbon black (2 vol.%). The thermoelectric power is increased from 8 to 163 μV/K, the electrical resistivity is decreased from 0.17 to 0.02.Ω.cm, the thermal conductivity is decreased from 1.31 to 0.51 W/m.K, and the dimensionless thermoelectric figure of merit ZT at 70 °C is increased from 9 × 10⁻⁶ to 9 × 10⁻². Tellurium increases the thermoelectric power greatly. Bismuth telluride decreases the electrical resistivity and thermal conductivity. Carbon black decreases the electrical resistivity.     

Potentiometric studies of N,N′-Bis(2-dimethylaminoethyl)-N,N′-dimethyl-9,10 anthracenedimethanamine as a chemical sensing material for Zn(II) ions

A liquid membrane based Zn²⁺ ion selective electrode containing N,N′-Bis(2-dimethylaminoethyl)-N,N′-dimethyl-9,10 anthracenedimethanamine (Bis(TMEDA) anthracene) (I) as ionophore has been prepared and characterized. The membrane comprises of PVC, ionophore and plasticizer in the ratio of 33:2:65, respectively. It showed the best response in terms of detection limit (1.5 × 10^− 6 M) and working concentration range (1.0 × 10^− 5 M to 1.0 × 10^− 1 M) with Nernstian response towards Zn²⁺ ions. The electrode responds within 15 s of coming in contact with the solution. The potential response remains almost unchanged over a pH range of 3.0 to 7.5. The electrode can be used for at least 3 months without any considerable alteration in its response behavior. The proposed electrode revealed good selectivity towards Zn²⁺ ions over a number of alkali, alkaline earth, transition metals and some other heavy metal ions. The electrode has been used as an indicator electrode in the potentiometric titration of Zn²⁺ with EDTA. The proposed electrode also detected Zn²⁺ ions from real life samples.     

Electronic transport properties of Fe-doped CoSb3 prepared by encapsulated induction melting

Fe-doped CoSb₃ skutterudites were prepared by encapsulated induction melting and their thermoelectric and electronic transport properties were investigated. The positive signs of Seebeck and Hall coefficients for all Fe-doped specimens revealed that Fe atoms successfully acted as p-type dopants by substituting Co atoms. Carrier concentration increased with increasing Fe doping content and the Fe dopants could affect the electronic structure of CoSb₃ and generate excess holes. However, carrier mobility decreased with increasing doping content, which indicates that the hole mean free path was reduced by the impurity scattering. Seebeck coefficient and electrical resistivity were almost independent of carrier concentration between 5.8 × 10¹⁹ and 2.0 × 10²⁰ cm^− 3 because the increase in carrier concentration by doping was competitive with the decrease in carrier mobility by the impurity scattering. Seebeck coefficient showed a positive value at all temperatures examined and it increased as the temperature increased. Temperature dependence of electrical resistivity suggested that Co_1 − xFe_xSb₃ is a highly degenerate semiconducting material. Thermal conductivity was considerably reduced by Fe doping and the lattice contribution was dominant in the Fe-doped CoSb₃ skutterudites.     

Fish protein hydrolysate production from sardine solid waste by crude pepsin enzymatic hydrolysis in a bioreactor coupled to an ultrafiltration unit

The aims of the study were to optimize the production a fish protein hydrolysate (FPH) by enzymatic hydrolysis of sardine solid waste using crude pepsin, and to scale up the process in a bioreactor coupled to an ultrafiltration unit for product recovery. Results showed that the crude pepsin prepared by autolysis of the mucous membranes of a sheep stomach at optimal conditions (i. e. pH = 1.5–2 and incubation time of 6 h) could be satisfactory used for the enzymatic hydrolysis of fish solid waste. The optimal conditions for enzymatic reaction were: temperature 48 °C, and pH 1.5. The scale up of the enzymatic hydrolysis and the coupling of the reactor an ultrafiltration unit to concentrate the hydrolysate gave good results with a rejection coefficient for the protein hydrolysate product in the range of 90%. The volumetric concentration factor was 2.5, with a permeate flux of 200 L m^? 2 bar^? 1. However, the results also suggest that the ultrafiltration product concentration process may be operating beyond the critical flux at which point irreversible membrane fouling occurs.     

Synthesis of Dy doped Yb0.1Ca0.9MnO3 ceramics with a high relative density and their thermoelectric properties

Perovskite-type Yb_0.1Ca_0.9?xDy_xMnO₃ ceramics were synthesized by solid state reaction. Their microstructures were characterized and the thermoelectric properties were evaluated between 300 K and 1100 K. Each of sample exhibits single phase with orthorhombic structure. All samples have high relative densities, and their values are between 95% and 97%, which is consistent with the SEM image. The electrical resistivity shows a typical metallic conductivity behavior. Lowest electrical resistivity 2.36 mΩ cm is achieved at room temperature, and the variation of electrical resistivity is not evident in whole measured temperature range. The Seebeck coefficients are negative, indicating an n-type conduction. The highest power factor 310 μW/(K² m) is obtained for the sample with x = 0.02. The thermal conductivity is decreased by the difference in the mass between the Ca²⁺ and Dy³⁺ ions, especially in the heavy doped samples. The highest figure of merit is 0.11 at 1069 K for the sample with x = 0.02.     

Role of Co–Cr substitution on the structural,electrical and magnetic properties of nickel nano-ferrites synthesized by the chemical co-precipitation method

Nano-spinel nickel ferrites doped with Co–Cr at iron and nickel sites are synthesized by the chemical co-precipitation method and are characterized by the XRD, DC electrical resistivity and hysteresis loops measurements. The XRD analyses confirm the formation of single spinel phase and the crystallite size calculated by Scherer's formula is found in the range of 17–19 nm. This crystallite size is small enough to obtain the suitable signal to noise ratio in the high density recording media. The values of electrical resistivity (8.28 × 10⁷ to 29.6 × 10⁷ ohm cm), activation energy (0.545–0.884 eV), saturation magnetization (23.67–33.49 emu g^?1) and remanence (12.48–18.67 emu g^?1) are increased up to a doping level of x = 0.2 and then starts to decrease. The increase in electrical resistivity, saturation magnetization and remanence suggest that the material with composition Co_0.2Ni_0.8Fe_1.8O₄ can be used for applications in microwave devices and high density recording media.     

Preparation and characterization of LTA-type zeolite framework dispersed ruthenium nanoparticles and their catalytic application in the hydrolytic dehydrogenation of ammonia–borane for efficient hydrogen generation

The safe and efficient hydrogen storage and production are major obstacles to use hydrogen as an energy carrier. Therefore, significant efforts have been focused on the development of new materials for the chemical hydrogen storage and production. Of particular importance, ammonia–borane (NH₃BH₃) is emerging as one of the most promising solid hydrogen carrier due to its high gravimetric hydrogen storage capacity (19.6 wt.%) and low molecular weight (30.8 g/mol). ammonia–borane can release hydrogen gas upon catalytic hydrolysis under mild conditions. Herein, the discovery of a new catalytic material, ruthenium nanoparticles stabilized by ZK-4 zeolite framework, for this important reaction has been reported. This new catalyst system was prepared by borohydride reduction of ruthenium(III)-exchanged ZK-4 zeolite in water at room temperature. The characterization of the resulting material by advanced analytical tools shows the formation of ZK-4 zeolite dispersed ruthenium nanoparticles (2.9 ± 0.9 nm). The catalytic performance of the resulting supported ruthenium nanoparticles depending on activity, lifetime and reusability was demonstrated in the hydrolytic dehydrogenation of ammonia–borane. They were found to be highly active (initial TOF = 5410 h^?1), long-lived (TTO = 36,700) and reusable catalyst (retaining of >85% of initial activity in the 5th reuse) in this important catalytic reaction at room temperature under air.     

Modification of UHMWPE by ion,electron and γ-ray irradiation

Due to good wear resistance Ultrahigh Molecular Weight Polyethylene (UHMWPE) is the material of choice for the load bearing surfaces of total joint implants. In order to improve its performance polymer parts are often modified by the use of ionizing radiation. Here we report on the use of electron and ion beams and γ-rays for the purpose. UHMWPE samples were irradiated with 600 keV and 1.5 MeV electron beam with doses ranging from 50 to 500 kGy and bombarded with 1–10 MeV He- and 9 MeV Cl-ions to fluences ranging from 10¹² to 5 × 10¹⁶ ions/cm². Co-bomb was used for γ-ray irradiation. Polymer radiolysis due to the irradiations was studied by means of nuclear reaction analysis (NRA) using the ¹H(¹⁵N, αγ)¹²C reaction. Hydrogen release increases with the applied dose and was correlated to the linear energy transfer (LET). Irradiated polymers oxidize rapidly when exposed to the air. Oxygen uptake profiles were determined using RBS. Correlation between radiolysis and oxidation has been revealed. Enriched in oxygen region extends to the depth at which radiation induced hydrogen release took place. Once started oxidation proceeds until the saturation concentration of about 10 at.% was attained.     

High performance cellulose acetate propionate composites reinforced with exfoliated graphene

This paper deals with the preparation, structural characterization, and physical performances of composites composed of biomass-based cellulose acetate propionate (CAP) and exfoliated graphene (EG). As a reinforcing nanofiller, EG is thus prepared by an oxidation/thermal expansion process of natural graphite flakes and it is characterized to consist of disordered graphene platelets. Structural features, thermal stability, mechanical modulus, and electrical resistivity of CAP/EG composites are investigated as a function of EG content. SEM and X-ray diffraction data demonstrate that graphene platelets of EG are well dispersed and exfoliated in the CAP matrix for the composites with up to ～1 wt.% EG, although they are partially aggregated in the composites with higher EG contents above ～3 wt.%. Thermo-oxidative stability of CAP/EG composites under active oxygen gas condition is improved substantially due to the gas barrier effect of graphene platelets of EG dispersed in the CAP matrix. Dynamic mechanical modulus of the composites is also enhanced significantly with increasing the EG content. This mechanical enhancement of CAP/EG composites is analyzed by adopting the Halpin–Tsai model. The electrical volume resistivity of CAP/EG composites prepared by melt-compounding is decreased dramatically from ～10¹⁵ to ～10⁶ Ω cm by forming the electrical conduction path at a certain EG content between 5 and 7 wt.%.     

High performance cellulose acetate propionate composites reinforced with exfoliated graphene

This paper deals with the preparation, structural characterization, and physical performances of composites composed of biomass-based cellulose acetate propionate (CAP) and exfoliated graphene (EG). As a reinforcing nanofiller, EG is thus prepared by an oxidation/thermal expansion process of natural graphite flakes and it is characterized to consist of disordered graphene platelets. Structural features, thermal stability, mechanical modulus, and electrical resistivity of CAP/EG composites are investigated as a function of EG content. SEM and X-ray diffraction data demonstrate that graphene platelets of EG are well dispersed and exfoliated in the CAP matrix for the composites with up to ∼1 wt.% EG, although they are partially aggregated in the composites with higher EG contents above ∼3 wt.%. Thermo-oxidative stability of CAP/EG composites under active oxygen gas condition is improved substantially due to the gas barrier effect of graphene platelets of EG dispersed in the CAP matrix. Dynamic mechanical modulus of the composites is also enhanced significantly with increasing the EG content. This mechanical enhancement of CAP/EG composites is analyzed by adopting the Halpin–Tsai model. The electrical volume resistivity of CAP/EG composites prepared by melt-compounding is decreased dramatically from ∼10¹⁵ to ∼10⁶ Ω cm by forming the electrical conduction path at a certain EG content between 5 and 7 wt.%.     

Equilibrium and kinetics of cadmium adsorption from aqueous solutions using untreated Pinus halepensis sawdust

Untreated Pinus halepensis sawdust has been investigated as an adsorbent for the removal of cadmium from aqueous solutions. Batch experiments were carried out to investigate the effect of pH, adsorbent dose, contact time, and metal concentration on sorption efficiency. The favorable pH for maximum cadmium adsorption was at 9.0. For the investigated cadmium concentrations (1–50 mg/L), maximum adsorption rates were achieved almost in the 10–20 min of contact. An adsorbent dose of 10 g/L was optimum for almost complete cadmium removal within 30 min from a 5 mg/L cadmium solution. For all contact times, an increase in cadmium concentration resulted in decrease in the percent cadmium removal (100–87%), and an increase in adsorption capacity (0.11–5.36 mg/g). The equilibrium adsorption data were best fitted with the Freundlich isotherm (R² = 0.960). The kinetics of cadmium adsorption was very well described by the pseudo-second-order kinetic model (R² > 0.999).     

AlCu alloy films prepared by the thermal diffusion technique

100-nm thick films of Al_1 ? xCu_x alloys were prepared on glass substrates by thermal diffusion technique. The Cu atomic concentration was varied from 10% to 90%. Alloys were prepared at different temperatures into a vacuum oven with Argon atmosphere. Two thermal processes were used: i) heating the film at 400 °C in a single step, and ii) heating the films in sequential steps at 100, 200, 300 and 400 °C. Morphology, electrical resistivity, and crystalline orientation of the alloys were studied. The electrical resistivity and surface roughness of the alloys were found to depend strongly on the atomic composition and the diffusion temperature. However, we did not find differences between samples prepared under the two thermal processes. Alloys prepared with x = 0.6 and x = 0.1–0.3 as Cu at concentration exhibited values on electrical resistivity and surface roughness lower than pure Al. Different phases of the Al_1 ? xCu_x films were observed as a function of Cu concentration showing a good agreement with the AlCu phase diagram.     

Gelation of photopolymerized hyaluronic acid grafted with glycidyl methacrylate

Experiments have tracked the ambient gelation of a series of hydrophilic hyaluronic acid (HA) resins grafted with glycidyl methacrylate (GM) and photopolymerized as a function of dose. The resin mixtures range in GMHA concentration between 0.5 and 1.5% w/w in phosphate buffered saline (PBS). Illuminated at 20 mW/cm², the dynamic viscosity (η(t)) has been tracked and characterized using the Boltzmann log-sigmoidal model. A gelled viscosity of ~ 10 Pa s was determined at 0.5% w/w which rose to ~ 50 Pa s at or above 1% w/w. More curing agent marginally increased the gel viscosity at each concentration. Time constants associated with viscosity advancement were shortest at [GMHA] = 1.0%; higher concentrations are attributed with lower quantum efficiency when illuminated. Subsequent frequency sweeps replicated already published work using similar GHMA concentrations in PBS. G′ values ranged from 100 to 500 Pa over the formulation range with expected sensitivity to GMHA and curing agent concentration. Overall, the sigmoidal model represented this advancing viscosity data well, and further analysis of the physical significance of these model parameters may help in understanding photopolymerization of this complicated formulation more broadly.