Synthesis of monodisperse and high-purity α-Si3N4 powder by carbothermal reduction and nitridation

Carbothermal reduction-nitridation method is an effective means for synthesizing Si₃N₄ powder. Herein, spherical monodisperse silica was used as silicon source. The effects of reaction temperature, nitrogen flow rate and Si₃N₄ seeds content on the products were studied. It was found that high-purity α-Si₃N₄ (>99.0 wt%) was synthesized from C/SiO₂ = 3:1 at 1400 °C, reaction time of 6 h and nitrogen flow rate of 800 ml/min. The powder, with an average size of 0.5 μm, showed good dispersity and regular morphology because spherical monodisperse silica could be completely coated with carbon. The more contact sites between SiO₂ and C, the higher concentration of SiO(g) would be produced in the initial stage. It also indicated that the nucleation rate of α-Si₃N₄ increased, thereby inhibiting the formation of an agglomerate phase and suppressing the grain growth of α-Si₃N₄. Furthermore, higher nitriding temperature and Si₃N₄ seeds content both decreased the grain size and increased β-Si₃N₄ content. The forming mechanism of non-agglomerated and submicron-sized α-Si₃N₄ was clarified.     

SiC/SiC and SiC/Kovar joining by Ni–Si and Mo interlayers

A composite joining technique, using a Ni–56Si filler alloy and Mo as interlayers, was used to join SiC to SiC and to Kovar. The wetting of the Ni–Si alloy on SiC ceramic was studied in a vacuum at 1,350 °C by the sessile drop technique as a function of time; the non-reactive wetting characteristics in the Ni–Si/SiC system were confirmed, with an equilibrium contact angle of about 23°. SiC/SiC joints were fabricated by two processes using a Ni–Si/Mo/Ni–Si structure as the interlayer. SiC/Kovar joints were produced by means of a multilayer structure: molybdenum, which is used as the interlayer, was joined to Kovar on one side by means of transient liquid phase bonding and to SiC on the other side, using a Ni–Si coating as a filler alloy. The resulting joints were analyzed and discussed in terms of joint morphology and microstructure, joint strength, and fracture behavior. Two interfacial layers form at the Kovar/Mo and the Mo/Ni–Si interfaces due to dissolution and interdiffusion phenomena between the metallic elements, without there being any observable reactions with the SiC component. The type of joining process and the experimental conditions used play a key role in determining the joint microstructure and composition, the joint strength and its fracture behavior.     

Synthesis of CuNbC nanocomposites by mechanical alloying

Elemental Cu and NbC powders were mechanically alloyed with either graphite or hexane to form nanocomposite CuNbC powders. These powders were consolidated by hotisostatic-pressing at one-third of the melting temperature of NbC to form a 100% dense compact, while maintaining a crystallite size well within the nano-regime.     

Synthesis,growth mechanism,photoluminescence and field emission properties of metal–semiconductor Zn–ZnO core–shell microcactuses

Metal–semiconductor Zn–ZnO core–shell microcactuses have been synthesized on Si substrate by simple thermal evaporation and condensation route using NH₃ as carrier gas at 600 °C under ambient pressure. Microcactuses with average size of 65–75 μm are composed of hollow microspheres with high density single crystalline ZnO rods. The structure, composition and morphology of the product were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscope (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). A vapor–liquid–solid (VLS) based growth mechanism was proposed for the formation of Zn–ZnO core–shell microcactuses. Room temperature photoluminescence (PL) investigations revealed a strong and broad blue emission band at 441 nm associated with a weak ultraviolet (UV) peak at 374 nm. This blue emission (BE) is different from usually reported green/yellow-green emission from Zn–ZnO or ZnO structures. The field emission (FE) measurements exhibited moderate values of turn-on and threshold fields compared with reported large field emissions for other materials. These studies indicate the promise of Zn–ZnO core–shell microcactuses for the applications in UV-blue light display and field emission microelectronic devices.     

Synthesis and characterization of V,Mo and Nb incorporated micro–mesoporous MCM-41 materials

Highly microporous metal-MCM-41 ordered mesoporous structure catalysts having different metal/Si (V, Mo, Nb) atomic ratios and combinations of metal sources were hydrothermally synthesized. The structural properties estimated using different techniques were found to be in agreement with each other. Metals were successfully incorporated into MCM-41 without deteriorating the ordered hexagonal structure. The metal ions in the synthesis solutions probably settled on the hydrophilic end of the template hence the metal incorporation resulted improvements in the micropore structure. Low loading of metals caused an increase in the surface area and pore volume values of the catalysts. The highest total (1310 m² g^?1) and micropore surface area values (1083 m² g^?1) were obtained by Nb incorporation. The micro- and mesopore dimensions of MCM-41 increased from 0.5 to 1.1 nm and from 2.5 to 2.8 nm, respectively, with metal incorporation. Low V/Si ratios and presence of Nb in the starting solution enhanced narrow mesopore size distribution. The pore dimension and wall thickness values estimated from nitrogen adsorption and X-ray diffraction methods were consistent with the corresponding values obtained using transmission electron microscopy.     

Synthesis of porous Mn3O4 microparticles by the KMnO4–AC reduction and combustion system

A direct method to synthesize porous hausmannite (Mn₃O₄) microparticles by the KMnO₄–AC reaction and combustion system is reported in this paper. In order to synthesize the manganese oxide, four experimental factors were considered: pH (3.0, 4.5 and 6.0), AC content (2.08 × 10^?2 and 8.33 × 10^?2 M), initial Mn(VII) content (4.55 × 10^?4 and 9.1 × 10^?4 M) and stirring velocity (300 and 500 rpm). The AC was added to the Mn(VII) aqueous solution and stirred for 2 h. For different pH levels, the Mn(VII) content in the solution was measured by UV/Vis spectrometry at 540 nm in order to evaluate the Mn reduction. Later, the manganese-loaded AC was calcined at 700°C in dry air at 1900 sccm during 60 min, indicating that the Mn₃O₄ content is directly proportional to the acidity of the solution. Spongy and porous Mn₃O₄ microparticles were synthesized considering the following levels: pH (3.0), an AC content (8.33 × 10^?2 M) and an initial Mn(VII) content (9.1 × 10^?4 M) with 500 rpm.     

Fabrication and mechanical evaluation of SiC–TiC nanocomposites by SPS

In the present study, the composites of SiC–TiC are prepared by spark plasma sintering (SPS) in vacuum without additive. The relationship of density and temperature of SiC–TiC composites with different content of TiC is studied. The maximum relative density reached was 98%. The mechanical properties of SiC–TiC composites with different content of TiC, which were sintered at 1800 °C, have been evaluated. From the fracture surface observation, two models of fracture mechanisms of the composites existed: transgranular and intergranular.     

Synthesis and characterization of NiO nanoparticles by sol–gel method

Nickel oxide nanoparticles have been synthesized in the presence of agarose polysaccharide by sol–gel method. The structure, morphology, optical and magnetic properties of the product was examined by X-ray diffraction, transmission electron microscopy, UV–visible spectrophotometer and superconducting quantum interference device magnetometer. The result of thermogravimetric analysis of the precursor product showed that the proper calcination temperature was 400 °C. X-ray diffraction result revealed that the obtained product was nickel oxide with face-centered cubic structure. TEM image demonstrated that the nickel oxide nanoparticles have spherical shape with size around 3 nm. Analysis of FTIR spectra confirmed the composition of product. The optical absorption band gap of the NiO nanoparticles was estimated to be 3.51 eV. Magnetic measurement showed that the nickel oxide nanoparticles exhibit superparamagnetic behavior at 300 K. Moreover, the nanoparticles show ferromagnetic interactions at 4.2 K owing to the existence of uncompensated moments on the surface of the nanoparticles.     

Phase evolution and reaction mechanism during reduction–nitridation process of titanium dioxide with ammonia

Titanium nitride powders were synthesized from titanium dioxide at 1173–1373 K in ammonia atmosphere. The reduction–nitridation products with various fractions obtained at various temperatures were analyzed by X-ray diffraction, Raman spectra, X-ray photoelectron spectroscopy, scanning electron microscope, transmission electron microscopy, and selected area electron diffraction. The reaction sequence from TiO₂ to TiN in ammonia atmosphere was changed by increasing the reaction temperature. The reaction sequence at 1173 K was found as TiO₂ → TiN_1?xO_x → TiN. When the reaction temperature was above 1273 K, the reaction sequence changed to as follows: TiO₂ → Ti₉O₁₇ → TiN_1?xO_x → TiN. Ti₃O₅ was not found as an intermediate phase on account of its instability in NH₃ atmosphere. The morphology of the synthesized TiN is closely related to that of the raw materials.     

Properties of carbon nano-tubes–Cf/SiC composite by precursor infiltration and pyrolysis process

Carbon nanotubes (CNTs) were introduced into the precursor infiltration and pyrolysis (PIP) carbon fiber reinforced silicon carbide matrix (C_f/SiC) composite via the infiltration slurry. The weight fraction of CNTs in the composite was 0.765‰. The fiber–matrix interface coating was prepared through chemical vapor deposition (CVD) process using methyltrichlorosilane (MTS). Effects of the CNTs on mechanical and thermal properties of the composite were evaluated by three-point bending test, single-edge notched beam (SENB) test, and laser flash method. Attributed to the introduction of the small quantity of CNTs, flexural strength and fracture toughness of the C_f/SiC composite both increased by 25%, and thermal conductivity at room temperature increased by 30%.     

Microstructure and strength of AlN–SiC interface studied by synchrotron X-rays

Bulk AlN crystals grown by sublimation on SiC substrates exhibit relatively high dislocation densities. The kind of defect formation at early growth stages influences the structural quality of the grown crystals. In this work, the dislocation distribution near to the interface is understood through investigation of thin (≤1.5 mm) continuous (non-cracked) freestanding crystals obtained in one process with the evaporation of the substrates. The AlN specimens were characterized using synchrotron radiation imaging techniques. We revealed by triple-axis X-ray diffraction study that, near to the former interface, randomly distributed dislocations configured to form boundaries between \(\sim \)0.02\(^{\circ }\) misoriented sub-grains (from [0001] direction). Threading dislocation structure similar to that in epitaxial GaN films was not detected. To explain these observations, a theoretical model of misfit stress relaxation near the interface is suggested.     

Effects of promoters on the product quality of nanophase SiC/α-Si3N4 composite powders synthesized through carbothermal reduction nitridation

The effect of additives is investigated for the carbothermal reduction synthesis of nanophase silicon carbide/silicon nitride composite powders. Mixtures of silica, carbon, seed silicon nitride, and additive are reacted in a thermogravimetric analyzer. The mass loss information combined with compositional and spectroscopic analysis allows product quality (morphology, surface area, -Si₃N₄ and -SiC contents, oxygen content, etc.) information to be obtained. It was observed that all of the additives used in this study increased the reaction rate. Lithium carbonate produced a silicon nitride/silicon carbide composite that was not significantly different from experiments without promoter. However, the product quality was severely affected in other instances.     

Dilatometric behavior and microstructure of sintered Fe–NbC and Fe–TaC composites

Fe-reinforced composites were manufactured by the addition of 10–20 wt.% NbC or TaC particles aiming at improved mechanical and wear behavior. Two varieties of Fe powders from Hoeganaes Corp. were used, Ancorsteel 1000B and 45P. Composites produced using the former variety included a small amount of Fe₃P to induce liquid-phase sintering whereas 45P powder was pre-alloyed with P by the manufacturer. The hardness of the matrix was adjusted adding carbon to the composite mixture. The powders were milled for different times and annealed prior to pressing. A dilatometric study was carried out under hydrogen to establish optimum sintering profiles. Relative densities up to 97% TD were achieved. Both microstructure and density of the sintered pellets were evaluated in order to establish correlations involving composition, processing parameters and microstructure of the composite.     

Synthesis of nanocrystalline AgPd alloys by chemical reduction method

Chemical reduction was used to produce nanocrystalline Ag-Pd alloy particles for applications in electronic component fabrication. The alloy particles were prepared at room temperature from formaldehyde-sodium hydroxide solutions and silver and palladium nitrates. Characterization of these particles by X-ray powder diffraction (XRD) reveals bi-metal and nanocrystalline silver-palladium alloys. Energy dispersive and XRD analysis of these products shows a complete range of solid solution. Characterization of the morphology, and the oxidation behavior of the Ag-Pd alloy powders are reported.     

Pulse and direct electrodeposition of Ni–Co/micro and nanosized SiO2 particles

Ni–Co/SiO₂ composite coating was electrodeposited on the steel substrate. The coatings were characterized by X-ray diffraction and scanning electron microscopy. The microhardness of the composite coatings was studied by variation of the electroplating parameters, such as the pulse current (PC) and direct current (DC) electrodeposition methods, deposition temperature, electrolyte pH, concentration of surfactants, sodium dodecyl sulfate (SDS), and cetyltrimethylammonium bromide (CTAB). Zeta potential of SiO₂ particles measurements was performed with various pH, SDS, and CTAB concentrations. The data depict that the hardness of Ni–Co/SiO₂ nanocomposite coatings manufactured by PC electrodeposition increases with the increase of bath temperature, pH, SDS, and CTAB concentration up to 50°C, 4.6, 0.3, and 0.2?g/L, respectively. Beyond mentioned optimum values, the microhardness of nanocomposite coating decreases. Using DC method led to reduce the microhardness. Utilizing SiO₂ microparticles instead of SiO₂ nanoparticles for reinforcing resulted in declining the microhardness. The friction coefficient and wear results demonstrated that using PC method and nanosized particles led to reduce the friction coefficient and increase the resistance to wear. Anodic polarization results illustrated that using SiO₂ nanoparticles and PC method to prepare coating caused corrosion resistance of coating in a 3.5?wt% NaCl solution to enhance.     

Synthesis of gold nanorods and nanowires by a microwave–polyol method

HAuCl₄ was reduced by ethylene glycol, in the presence of polyvinylpyrrolidone (PVP) under microwave (MW) heating in a continuous wave (CW) mode for 2 min. Dominant products were polygonal nanoplates and close-to-spherical nanoparticles of gold. In addition, small amounts of single crystalline gold nanorods and nanowires (0.5–3% of total number of products) with diameters of 20–100 nm and lengths of 0.6–5 μm were produced. The diameter and length of gold nanorods and nanowires could be controlled by changing the HAuCl₄·4H₂O/PVP ratio. The formation mechanism of anisotropic gold nanostructures was discussed.     

Synthesis and processing of ceramic–metal composites by reactive metal penetration

Molten aluminum reduces and penetrates silicate ceramics to produce a metal–ceramic composite which yields an Al₂O₃ skeleton infiltrated with a solidified Al–Si alloy. Penetration experiments have been used to study the influence of p(O₂), temperature and substrate composition on penetration kinetics and composite microstructure. The limiting kinetic step for Al penetration is the chemical reaction between Al and the ceramic. For dense substrates the maximum reaction rates are observed between 1000–1200°C and are independent of p(O₂). For porous substrates it is necessary to reach a critical temperature or p(O₂), before infiltration starts. Increasing the Si concentration in the molten Al results in the reduction of the reaction rates.     

Influence of coal tar pitch coating on the properties of micro and nano SiC incorporated carbon–ceramic composites

Carbon-micro or nano silicon carbide–boron carbide (C-micro or nanoSiC–B₄C) composites were prepared by heating the mixtures of green coke and carbon black as carbon source, boron carbide and silicon at temperature of 1,400 °C. Green coke reacts with silicon to give micron sized silicon carbide while the reaction between silicon and carbon black gives nano silicon carbide in the resulting carbon–ceramic composites. The green coke was coated with a suitable coal tar pitch material and used to develop carbon-(micro or nano) silicon carbide–boron carbide composites in a separate lot. The composites were characterized for various properties including oxidation resistance. It was observed that both types of composites made from uncoated as well as pitch-coated green coke exhibited good oxidation resistance at 800–1,200 °C. The density and bending strength of composites developed with pitch-coated green coke improved significantly due to the enhanced binding of the constituents by the pitch.