Determination of the types of nitrogen in steels containing aluminium or titanium by an extraction method with hydrogen

The extraction method with hydrogen, hitherto used to determine mobile nitrogen in steels over the temperature range 350–450°C, has been employed at higher temperatures to determine nitrogen bound as aluminium nitride, or as titanium nitride or carbonitride. In steels containing only silicon and titanium as deoxidizers, the nitrogen remaining after passage of hydrogen at 600 or 750°C is present as titanium nitride or carbonitride and can be determined by difference. In steels containing only silicon and aluminium as deoxidizers, the nitrogen remaining after passage of hydrogen at 600°C is present as aluminium nitride and can also be determined by difference. This was verified by determining the aluminium nitride indirectly. The nitrogen released from both the aluminium and titanium steels in hydrogen at 600°C probably results from dissociation of submicroscopic particles of manganese silicon nitride.     

Evaluation of interlaminar fracture toughness and dynamic mechanical properties of nano TiO2 coated flax fibre epoxy composites

In this study, fibre modification technique is performed by coating nano titanium dioxide (TiO₂) particles on flax fibres. The fibre surface is treated with silane coupling agents and coated with nanoparticles at weight percentage 0.2, 0.4, 0.6 and 0.8% to develop chemical bonding at the fibre matrix interface. The improved interface is evaluated by performing Mode I, Mode II interlaminar fracture toughness (ILFT), and Dynamic mechanical analysis (DMA). The results indicate that the fibre modified composites with 0.4 wt % and 0.6 wt % coating shows 37% and 24% improvement in Mode I and Mode II ILFT values respectively. The storage modulus from the DMA analysis also exhibits improvement for the fibre modified composites. SEM analysis explains the changes in the fracture mechanism. FTIR analysis provides the details on the fibre coating by nanoparticles.     

Photocatalytic Activity of Titanium Dioxide Nanoparticles Immobilized in the Polymer Network of Polyacrylamide Hydrogel

Composite hydrogels based on polyacrylamide immobilized nanoparticles of commercial (P25 brand) titanium dioxide and of titanium dioxide nanoparticles prepared by electric explosion of a wire were synthesized. The enthalpy of interaction at the polyacrylamide/TiO₂ interface was determined by microcalorimetry using the thermochemical cycle method. Interaction of polyacrylamide polymer chains with the surface of TiO₂ nanoparticles is energetically unfavorable. The absence of interactions between the hydrogel polymer network and surface of TiO₂ nanoparticles favors manifestation of the UV-induced photocatalytic activity of TiO₂ nanoparticles immobilized in the hydrogel. Immobilization in the polyacrylamide hydrogel matrix decreases the photocatalytic activity of P25 brand TiO₂ nanoparticles, but does not affect the photocatalytic activity of titanium dioxide nanoparticles prepared by the electric explosion method. The photocatalytic activity of TiO₂ nanoparticles immobilized in the bulk of polyacrylamide hydrogel evaluated by the decomposition of Methyl Orange dye is controlled by the diffusion rate of the dye molecules into the bulk of the hydrogel and depends also on the aggregation of TiO₂ nanoparticles in the hydrogel matrix.

     

Pulsed TEA CO2 Laser Irradiation of Titanium in Nitrogen and Carbon Dioxide Gases

Surface changes created by interaction of transversely excited atmospheric carbon dioxide (TEA CO₂) laser with titanium target/implant in nitrogen and carbon dioxide gas were studied. TEA CO₂ laser operated at 10.6 μm, pulse length of 100 ns and fluence of ∼17 J/cm² which was sufficient for inducing surface modifications. Induced changes depend on the gas used. In both gases the grain structure was produced (central irradiated zone) but its forms were diverse, (N₂: irregular shape; CO₂: hill-like forms). Hydrodynamic features at peripheral zone, like resolidified droplets, were recorded only in CO₂ gas. Elemental analysis of the titanium target surface indicated that under a nitrogen atmosphere surface nitridation occurred. In addition, irradiation in both gases was followed by appearance of plasma in front of the target. The existence of plasma indicates relatively high temperatures created above the target surface offering a sterilizing effect.

     

Electron Microscopy Characterization of Silicon Dioxide Nanotubes

Well‐developed crystals of [Pt(NH₃)₄](HCO₃)₂ are employed as template for the synthesis of silicon dioxide nanotubes (SiO₂‐NTs). Silicon dioxide, which is produced by a sol‐gel reaction, coats the surface of these crystals and builds up the nanotube walls. In the final step, the Pt‐salt fibers are thermally decomposed and auto‐reduced to metallic Pt nanoparticles. Scanning and transmission electron microscopy (SEM and TEM) investigations of the product confirm the formation of silicon dioxide nanotubes in high yield. The tube walls consist of amorphous silicon dioxide. The tube length generally is 0.5 — 3 μm, while the thickness varies in two distinct ranges: thick tubes have a diameter of 100 — 500 nm and thin ones of approximately 50 nm. Most of the NTs are filled with Pt particles, but others, typically the larger ones with open tube ends, obviously are empty. Presumably, open ends cause the observed Pt loss. In closed SiO₂‐NTs, Pt forms as ca. 10 nm large particles in the tube core and as 1 — 2 nm large particles inside the tube walls.     

XPS study on the use of 3-aminopropyltriethoxysilane to bond chitosan to a titanium surface

Chitosan, a biopolymer found in the exoskeletons of shellfish, has been shown to be antibacterial, biodegradable, osteoconductive, and has the ability to promote organized bone formation. These properties make chitosan an ideal material for use as a bioactive coating on medical implant materials. In this study, coatings made from 86.4% de-acetylated chitosan were bound to implant-quality titanium. The chitosan films were bound through a three-step process that involved the deposition of 3-aminopropyltriethoxysilane (APTES) in toluene, followed by a reaction between the amine end of APTES with gluteraldehyde, and finally, a reaction between the aldehyde end of gluteraldehyde and chitosan. Two different metal treatments were examined to determine if major differences in the ability to bind chitosan could be seen. X-ray photoelectron spectroscopy (XPS) was used to examine the surface of the titanium metal and to study the individual reaction steps. The changes to the titanium surface were consistent with the anticipated reaction steps, with significant changes in the amounts of nitrogen, silicon, and titanium that were present. It was demonstrated that more APTES was bound to the piranha-treated titanium surface as compared to the passivated titanium surface, based on the amounts of titanium, carbon, nitrogen, and silicon that were present. The metal treatments did not affect the chemistry of the chitosan films. Using toluene to bond APTES on titanium surfaces, rather than aqueous solutions, prevented the formation of unwanted polysiloxanes and increased the amount of silane on the surface for forming bonds to the chitosan films. Qualitatively, the films were more strongly attached to the titanium surfaces after using toluene, which could withstand the ultrahigh vacuum environment of XPS, as compared to the aqueous solutions, which were removed from the titanium surface when exposed to the ultrahigh vacuum environment of XPS.     

Bactericidal activity and UV-filtering property of TiO<Subscript>2</Subscript>-based photocatalysts coated on curtain fabrics

Synthesized and commercial titanium dioxide (TiO₂) were coated onto household curtain fabrics for anti-microbial and ultraviolet (UV) shielding functions. The coating was performed by inducing a deposition of the TiO₂ layer from the Ti precursor onto the fabric surface. A silane adhesive agent was employed to improve the adhesion between the coating and the fabric. Ag nanoparticles were also incorporated into some samples to further improve the anti-bacterial activity, which was evaluated by a standard qualitative test (AATCC 147). Efficiency for UV shielding was evaluated by measuring a UV–visible reflection of the coated fabrics both before and after subjecting it to several washing cycles. The results showed that the TiO₂-coated fabrics had potential as both anti-bacterial and UV shielding for the curtain industry.     

Enhancement of Germination and Seedling Growth of Wheat Seed Using Dielectric Barrier Discharge Plasma with Various Gas Sources

The influences of non-thermal discharge plasma treatment on wheat seed germination and seedling growth were investigated using a dielectric barrier discharge (DBD) plasma system at atmospheric pressure and room temperature. DBD plasma with various gas sources (oxygen, air, argon, and nitrogen) was employed in this study. Germination characteristics, seedling growth parameters, surface changes of the seed coat, permeability, and soluble protein of the seedlings were measured after the DBD plasma treatments. The experimental results showed that moderate-intensity DBD plasma had active impacts on wheat seed germination and seedling growth. Germination potential significantly increased by 24.0, 28.0, and 35.5% after 4 min of the air plasma, nitrogen plasma, and argon plasma treatments, respectively, compared with the control; and the shoot and root length also increased; however, no enhancement was observed after the oxygen plasma treatment. Scanning electron microscope analysis showed that etching effects on the seed coat occurred after the air plasma, nitrogen plasma, and argon plasma treatments, which affected the hygroscopicity and permeability of the wheat seed. In addition, moderate-intensity DBD plasma could also activate several physiological reactions in wheat seed, resulting in the increase of soluble protein production in wheat seedlings.     

Effect of the Titanium Dioxide Shell on the Plasmon Properties of Silver Nanoparticles

The results of the synthesis of Ag—TiO₂ nanostructures were presented. The optical properties of silver nanoparticles and Ag—TiO₂ structures were studied. The size and shape of Ag—TiO₂ nanostructures were determined. The electron density in silver, the damping constant of plasma oscillations, and the ratio between the masses of the Ag core and the TiO₂ shell were determined from the absorption spectra of Ag and Ag—TiO₂ solutions. It was shown that the semiconductor shell of titanium dioxide leads to a decrease in the electron density in silver nanoparticles and the damping constant of plasma oscillations.     

Sol‐Gel‐Process in the Ammono‐System – a Novel Access to Silicon Based Nitrides

Controlled coammonolysis of elementalkylamides in aprotic organic solvents at low temperatures have been shown to result in the formation of polyazanes. The synthetic procedure developed may be addressed as “sol‐gel‐route in the ammono system”. Pyrolysis of these novel polymer precursors gave access to multinary nitrides. For the model systems Si(NHMe)₄/B(NMe₂)₃, Si(NHMe)₄/Ti(NMe₂)₄, and Si(NHMe)₄/Ta(NMe₂)₅ polymeric boro‐, titano and tantalosilazanes were obtained. Pyrolysis in ammonia at 1000 °C yielded amorphous silicon boron nitride, silicon titanium nitride and silicon tantalum nitride powders; further heating of the nitride powders at 1500 °C in nitrogen atmosphere led to the formation of partly crystalline composites of α‐Si₃N₄ and amorphous silicon boron nitride for the Si/B/N system, a composite of finely dispersed TiN and amorphous silicon titanium nitride for the Si/Ti/N system, and crystalline TaN and amorphous silicon nitride for the Si/Ta/N system. Furthermore, the structure and pyrolysis chemistry of the polymeric intermediates, as well as the morphology of the pyrolysis products, were studied by NMR, MAS‐NMR, FT‐IR, DTA‐TG‐MS, XRD, SEM, EDX and elemental analyses.     

Thermochemistry of thermal plasma chemical reactions. Part II. A survey of synthesis routes for silicon nitride production

Feasibility routes for thermal plasma production of silicon nitride powders are explored. First, a collation of the various proposed systems from the extant literature is examined. Reactant systems investigated include free silicon, silicon monoxide, silicon dioxide, silicon tetrachloride, silane, and other organosilicon precursors, along with various nitriding and reducing species. The reaction yields of these systems are brought to a common denominator by thermodynamic analysis and a first-step introduction of nucleation kinetics including comparisons against published experiments and the authors' own research. In particular, it is observed that the formation of liquid-phase free silicon in the neighborhood of 2500 K is quite detrimental to silicon nitride yield, and furthermore, a high supersaturation of silicon should always be avoided.     

DBD Plasma Treatment of Titanium in O2, N2 and Air

Dielectric Barrier Discharge plasma treatment of a titanium metal foil in oxygen, nitrogen and air under atmospheric conditions is investigated employing X-Ray Photoelectron Spectroscopy (XPS). We investigated three different reference samples and compare the results with a large number of studies on the XPS analysis of titanium compounds containing oxygen and nitrogen. The plasma treatment in all three different process gases leads to the formation of titanium dioxide films, while rather small nitrogen fractions are found after nitrogen and air plasma treatments. This finding is explained basing on plasma chemistry insight from the literature.     

Synthesis of titanium nitride and carbonitride nanopowders in confined-jet flow plasma reactor

The synthesis of titanium nitride and carbonitride nanopowders from titanium tetrachloride vapor in a stream of hydrogen–nitrogen plasma, generated by an arc torch, in confined-jet flow reactor has been experimentally studied. Single-phase nanopowders with a NaCl-type cubic crystal lattice as assemblies of preferably cube-shaped nanoparticles of a 20–150 nm size and aggregates based on them have been obtained in the experiments. By varying the synthesis parameters, it has been possible to prepare titanium nitride nanopowders with a specific surface area in the range of 11–39 m²/g containing 18.8–22.5 wt % nitrogen, which corresponds to the empirical formula TiN_0.79–TiN_0.99. The titanium carbonitride nanopowders had a specific surface area of 13–23 m²/g and carbon and nitrogen contents of 7.5–13.6 and 13.5–5.1 wt %, respectively.     

Surface and interface analysis of titanium nitride diffusion barriers

Titanium nitride films were produced on silicon substrate by ion beam assisted deposition in the alternate mode: first, thin titanium layers were deposited by electron beam evaporation and then titanium nitride was formed by nitrogen implantation at room temperature; this cycle was then iterated many times in order to obtain thicker titanium nitride layers. The obtained films were characterized with respect to atomic composition by Rutherford backscattering spectrometry and nuclear reaction analysis techniques, while chemical bonding was investigated by Auger line-shape analysis. We observe that nitrogen implantation, along with the production of titanium nitride, induces silicon migration into the film. Silicon transport is connected to point defects produced by ion implantation as well as by chemical driving forces associated with silicides formation.     

重量法-电感耦合等离子体原子发射光谱法联用测定无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量

二氧化硅是无取向硅钢环保涂层液的核心成分,其含量直接影响硅钢涂层的固化工艺及涂层产品的磁性能。因此为保证涂覆过程的顺利进行,对涂层液中二氧化硅含量的检测是十分必要的。本方法采用样品中分别加入硝酸、双氧水及高氯酸,置于电热板上进行消解处理,处理后的样品经酸溶、过滤步骤,以重量法计算沉淀中二氧化硅的含量,采用电感耦合等离子体原子发射光谱（ICP-AES）仪测定滤液中可溶性硅含量,则样品中二氧化硅含量为重量法和电感耦合等离子体原子发射光谱法测定结果的合量。从而建立了重量法-电感耦合等离子体原子发射光谱法联用测定无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量的方法。讨论了样品前处理用消解酸及消解温度、滤液中可溶性硅及含量、ICP-AES仪器检测时的元素干扰。结果表明：按照本实验方法测定无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量,检测结果的相对标准偏差（RSD,n=12）在0.76%~1.08%之间,加标回收率在97.00%~104.0%之间。该方法可广泛应用于各检测部门对无取向硅钢磷酸盐体系环保涂层液中二氧化硅含量的监控。     

Penetration Study of Formulated Nanosized Titanium Dioxide in Models of Damaged and Sun‐Irradiated Skins

Inorganic ultraviolet filters such as titanium dioxide (TiO₂), safe to use on healthy skin, are often applied on compromised and irradiated skin. The aim of this study was to evaluate in vitro the cutaneous penetration of TiO₂ nanoparticles (≥ 20 nm primary size), included in a sunscreen, in intact, damaged, irradiated, and damaged/irradiated pigskin. Cutaneous penetration and localization of TiO₂ after a 24‐h sunscreen application were investigated quantitatively using inductively coupled plasma‐mass spectrometry, and qualitatively using transmission electron microscopy (TEM). Elemental identity of the nanoparticles was evaluated by TEM‐coupled Energy Dispersive X‐ray analysis (TEM‐EDX). In intact and damaged/irradiated skins, 102.35 ± 4.20% and 102.84 ± 5.67% of the titanium deposited, respectively, were found at the surface and stratum corneum (SC), whereas only 0.19 ± 0.15% and 0.39 ± 0.39% were found in the viable epidermis and dermis and no titanium was detected in the receptor fluid. TEM‐EDX analysis confirmed the presence of titanium in the aggregates formed by TiO₂ at the SC surface, as already characterized in the sunscreen formulation. TiO₂ nanoparticles included in a sunscreen thus remain in the uppermost layers of the SC, whether in intact skin or in compromised and/or skin exposed to simulated solar radiation.     

Wet Conversion of Methane and Carbon Dioxide in a DBD Reactor

The influence of water on the plasma assisted conversion of methane and carbon dioxide in a dielectric barrier discharge (DBD) plug flow reactor was studied. The plasma at atmospheric pressure was ignited by a power supply at a frequency of 13.56?MHz. Product formation was studied at a power range between 35 and 70?W. The concentrations of the three gases were altered and diluted with helium to 3?%. FTIR spectroscopy and mass spectroscopy were applied to analyze the inlet and the product streams. The main product of this process are hydrogen, carbon monoxide and ethane. Ethene, ethine, methanol and formaldehyde are generated beside the main products in this DBD in lower concentrations. The conversion of methane, the ratio of the synthesis gas components (n(H₂):n(CO)), and the yield of oxygenated hydrocarbons and hydrogen increases by adding water. The total consumed energy reaches lower values for small amounts of water. Additional water does not influence the generated amount of C2 hydrocarbons and of CO, but decreases the carbon dioxide conversion.     

Synthesis of Functional Oxide Nanoparticles Through RF Thermal Plasma Processing

A method of synthesizing functional nanostructured powders through reactive thermal plasma processing has been developed. Nano-sized oxide powders, including titanium dioxide and some functional oxides, were synthesized by the oxidation of liquid precursors. Oxides with the prescribed cation ratio of the liquid precursor can be synthesized with this technique, and it is possible to precisely adjust the chemical composition, which is linked to the appropriate functions of ceramic materials. Quench gases, either injected from the shoulder of the reactor or injected counter to the plasma plume from the bottom of the reactor, were used to vary the quench rate; therefore, the particle size of the resultant powders. The experimental results are well supported by numerical analysis on the effects of quench gases on the flow pattern and temperature field of thermal plasma as well as on the trajectory and temperature history of particles. Plasma-synthesized TiO₂ nanoparticles showed phase preferences different from those synthesized by conventional wet-chemical processes. Nano-sized particles of high crystallinity and nonequilibrium chemical composition were formed in one step via reactive thermal plasma processing. The plasma-synthesized nanoparticles were spherical and hardly agglomerated, and high dispersion properties were observed, i.e., the plasma-synthesized TiO₂ nanoparticles were individually dispersed in water.     

Synthesis of platinum nanoparticles on substrates of various chemical natures using supercritical carbon dioxide

A method for synthesizing platinum nanoparticles on a dispersed substrate using supercritical carbon dioxide was applied on substrates of various chemical natures: silicon carbide, titanium nitride, and tin dioxide. On all the substrates, materials with narrow uniform platinum nanoparticle size distributions were obtained. The platinum nanoparticle size distribution on each of the substrates was studied. It was shown that the platinum particle sizes are within a narrow range with an average particle size of about 3 nm and scarcely dependent on the chemical nature of the substrate.     

Methane Conversion to Higher Hydrocarbons in the Presence of Carbon Dioxide Using Dielectric-Barrier Discharge Plasmas

Experimental investigation has been conducted to convert methane into higher hydrocarbons in the presence of carbon dioxide within dielectric-barrier discharge (DBD) plasmas. The objectives of cofeed of carbon dioxide are to inhibit carbon deposit and to increase methane conversion. The products from this plasma methane conversion include: (1) syngas (H₂+CO), (2) gaseous hydrocarbons containing ethylene, acetylene, and propylene, (3) liquid hydrocarbons, (4) plasma-polymerized film, and (5) oxygenates. The selectivity of products is subject to the DBD plasma-reactive conditions and catalyst applied. The liquid hydrocarbons produced by this way are highly branched, which represents a better fuel production.