Crystallization of an amorphous B–C–N precursor with a Li–B–N catalyst at high pressures and temperatures

An orthorhombic B–C–N compound was synthesized using an amorphous B–C–N precursor and a Li–B–N catalyst at 6 GPa and 1773 K. The results of energy dispersive spectrometry and electronic energy loss spectrometry suggest a stoichiometry of B:C:N = 1:3.3:1. In addition, the Li–B–N catalyst improves the crystallizations of the B–C–N compound, graphite and BN and therefore might be a profitable catalyst in ultrahigh pressure experiments.     

Characterization of transient-liquid-phase-bonded joints in a duplex stainless steel with a Ni–Cr–B insert alloy

Transient liquid-phase bonding of a duplex stainless steel was performed with a Ni–Cr–B insert alloy. The microstructure of the joint region was investigated by cross-sectional and layer-by-layer characterization. According to the experimental studies, prior to completion of isothermal solidification, the bond microstructure can be expressed as γ-Fe + δ-Fe/γ-Fe + δ-Fe + BN/γ-Ni(Fe) + BN/γ-Ni + Cr-rich borides/γ-Ni + Ni₃B + Cr-rich borides (CrB, CrB₂, Cr₂B₃, Cr₃B₄, Cr₅B₃ and CrB₄), from the base metal side to the bonded-interlayer side. Complete isothermal solidification occurred at 1090 °C within 3600 s. Only the γ-Ni solid solution phase was present in the bonded interlayer, and BN precipitates were not removed after isothermal solidification. The formation of secondary-phase precipitates might be responsible for the presence of peak microindentation hardness in the bond region.     

Solidification microstructures and mechanical properties of high-vanadium Fe–C–V and Fe–C–V–Si alloys

Fe–C–V and Fe–C–V–Si alloys of various C, V and Si compositions were investigated in this work. It was found that the phases present in both of these alloy systems were alloyed ferrite, alloyed cementite, and VC_x carbides. Depending on the alloy composition the solidified microstructural constituents were granular pearlite-like, lamellar pearlite, or mixtures of alloyed ferrite + granular pearlite-like or granular pearlite-like + lamellar pearlite. In addition, it is shown that in Fe–C–V alloys the C/V ratio influences (a) the type of matrix, (b) the fraction of vanadium carbides, f_v and (c) the eutectic cell count, N_F. In Fe–C–V alloys, a relationship between the alloy content corresponding to the eutectic line was experimentally determined and can be described by where C_e and V_e are the carbon and vanadium composition of the eutectic. Moreover, in the Fe–C–V alloys (depending on the alloy chemistry), the primary VC_x carbides crystallize with non-faceted or non-faceted/faceted interfaces, while the eutectic morphology is non-faceted/non-faceted with regular fiber-like structures, or it possesses a dual morphology (non-faceted/non-faceted with regular fiber-like structures + non-faceted/faceted with complex regular structures). In the Fe–C–V–Si system, the primary VC_x carbides solidify with a non-faceted/faceted interface, while the eutectic is non-faceted/faceted with complex regular structures. In particular, spiral eutectic growth is observed when Si is present in the Fe–C–V alloys. In general, it is found that as the matrix constituent shifts from predominantly ferrite to lamellar pearlite, the hardness, yield and tensile strengths exhibit substantial increases at expenses of ductility. Moreover, Si additions lead to alloy strengthening by solid solution hardening of the ferrite phase and/or through a reduction in the eutectic fiber spacings with a decrease in the alloy ductility.     

Characterization of precipitates in a 7.9Cr–1.65Mo–1.25Si–1.2V steel during tempering

In this paper, the precipitates formed during the tempering after quenching from temperature 1150 °C for 7.90Cr–1.65Mo–1.25Si–1.2V steels are investigated using an analytical transmission electron microscope (A-TEM).The study of this tempering is carried out in isothermal and anisothermal conditions, by comparing the results given by dilatometry and hot hardness.Tempering is performed in the range of 300–700 °C. Coarse primary carbides retained after heat treatment are V-rich MC and Cr–Mo-rich M₇C₃ types. In turn, it gives a significant influence on the precipitation of fine secondary carbides, that is, secondary hardening during tempering. The major secondary carbides are Cr–Mo–V-rich M′C (and/or) Cr–Mo-rich M₂C type. The peak hardness is observed in the tempering range of 450–500 °C. In the end, we observe between 600 and 700 °C, that this impoverished changes the phase. At these high temperatures of tempering, we observe that there is a carbide formation of the types M₆C developing at the expense of the fine M₇C₃ carbides previously formed.     

Ni–Zr–Ti–Si–Sn/Cu metallic glass composites prepared by magnetic compaction

Ni–Zr–Ti–Si–Sn/Cu metallic glass (BMG) composites were fabricated by magnetic compaction of powder mixtures. A considerable plastic deformation took place without apparent failure during the dynamic compaction even at room temperature and at a high strain rate. The BMG particles retained their amorphous phase after the dynamic magnetic compaction at 450 °C. The resulting Ni_52.65Zr_28.71Ti_13.57Si_1.33Sn_3.74/60% Cu composite exhibited a remarkable tensile ductility at room temperature combined with high strength: tensile elongation of 28% and ultimate tensile stress up to 1.1 GPa.     

Preparation and photoluminescence properties of ZnO/amorphous-BaTiO3 thin-films by sol–gel process

ZnO/amorphous-BaTiO₃ thin-films were prepared on glass substrates by a sol–gel process. DSC/TGA, XRD and AFM were used to analyze the thermolysis of the precursor and the crystal growth characteristics of ZnO, and IR spectroscopy was used to determine the presence of OH groups and CO impurities containing in the films. Violet emission centering at 418 and 438 nm was observed in room temperature PL spectra of the films annealed at 400–500 °C. The strongest violet emission was observed in the film annealed at 400 °C. The emission intensity reduces as the annealing temperature increases, and vanishes in the film annealed at 550 °C. All of the films contain OH and CO groups, and the films annealed at the temperature over 450 °C contain CO₂ impurities, indicating the enhancing oxidation of the films. The vanishing of the violet emission is probably due to the improvement of the oxygen deficient of ZnO crystals.     

Crystallization and oxidation resistance properties of boron modified silicon oxycarbides derived from polymeric precursors by sol–gel method

Boron modified silicon oxycarbides (SiBOCs) were prepared from sol–gel derived pre-ceramic polymeric gels followed by pyrolysis at 950 °C under nitrogen. As-prepared SiBOC was found to be amorphous in nature and partially crystallized to SiO₂ at 1500 °C. The effect of boron incorporation on the crystallization of SiBOC was studied and the result revealed that the tendency to crystallization decreased with increasing boron content. This is due to the formation of Si–O–B bridges at higher temperatures, which retards the crystallization of SiO₂, evidenced from FTIR studies. SiBOC also exhibited excellent oxidation resistance ability at high temperature.     

Physical properties of transparent conducting Cd–Te–In–O thin films: Outlining a thermodynamic system for transparent conducting oxides

Cd–Te–In–O thin films are grown by pulsed laser deposition using a composite target of CdTe powder embedded in an indium matrix. Oxygen pressures range from 2.00 to 6.67 Pa at a substrate temperature of 420 °C. The structure, optical transmission and sheet resistance of the films are measured. Substitutional compounds with In_2 − 2x(Cd,Te)_2xO₃ stoichiometry are found at high oxygen pressures. A ternary phase diagram of the CdO–In₂O₃–TeO₂ system shows the relationship between the structure and the stoichiometry of the films. To evaluate film performance, a figure of merit is proposed based on the relationship between the integral photonic flux and the sheet resistance. The best figure of merit values corresponds to a sample prepared at 3.8 Pa O₂ that consists of (In₂O₃)_0.3(CdTe₂O₅)_0.7 and exhibits an optical band gap of 3.0 eV. This sample is a suitable substrate for electrodeposition due to its good electrochemical stability.     

Effect of rapid solidification on the microstructure and mechanical properties of hot-pressed Al–20Si–5Fe alloys

The aim of this work is to study the effect of cooling rate and subsequent hot consolidation on the microstructural features and mechanical strength of Al–20Si–5Fe–2X (X = Cu, Ni and Cr) alloys. Powder and ribbons were produced by gas atomization and melt spinning processes at two different cooling rates of 1 × 10⁵ K/s and 5 × 10⁷ K/s. The microstructure of the products was examined using optical microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The particles were consolidated by hot pressing at 400 °C/250 MPa/1 h under a high purity argon atmosphere and the microstructure, hardness and compressive strength of the compacts were evaluated. Results showed a profound effect of the cooling rate, consolidation stage, and transition metals on the microstructure and mechanical strength of Al–20Si–5Fe alloys. While microstructural refining was obtained at both cooling rates, the microstructure of the atomized powder exhibited the formation of fine primary silicon (~ 1 μm), eutectic Al–Si phase with eutectic spacing of ~ 300 nm, and δ-iron intermetallic. Supersaturated Al matrix containing 5–7 at.% silicon and nanometric Si precipitates (20–40 nm) were determined in the microstructure of the melt-spun ribbons. The hot consolidation resulted in coarsening of Si particles in the atomized particles, and precipitation of Si and Fe-containing intermetallics from the supersaturated Al matrix in the ribbons. The consolidated ribbons exhibited higher mechanical strength compared to the atomized powders, particularly at elevated temperatures. The positive influence of the transition metals on the thermal stability of the Al–20Si–5Fe alloy was noticed, particularly in the Ni-containing alloy.     

Optimization of PVD Parameters for the Deposition of Ultrahard Ti–Si–B–N Coatings

Multicomponent Ti–Si–B–N coatings were deposited on high-speed steel (HSS) substrates by reactive magnetron sputtering using a SHS TiB + 20 wt% Si target. The influences of the substrate temperature, bias voltage, and nitrogen partial pressure on the structure and the elemental compositions of the films were studied. The films were characterized by high-resolution transmission electron microscopy (HRTEM), Auger spectroscopy (AES), and X-ray diffraction (XRD). The results of HRTEM analysis indicated the formation of an ordered–disordered structure with fine crystalline grains of hexagonal Ti(B,N) _x phase and amorphous integrain layers. The stoichiometry of the Ti(B,N) _x phase was strongly affected by PVD process parameters. The films were characterized in terms of their microhardness and wear resistance. The reasons for the high value of microhardness appear to be the result of stoichiometric phase composition, compressive residual stress, and dense and fine microstructure of the Ti–Si–B–N coatings. The tribological wear test results indicated the superior wear-resistant properties of Ti–Si–B–N coatings compared to TiN and Ti(C,N) coatings.     

Rapid densification and reaction sequences in self-reinforced Y-α-SiAlON ceramics with barium aluminosilicate as an additive

Y-α-SiAlON (Y_1/3Si₁₀Al₂ON₁₅) ceramics with 5 wt.%BaAl₂Si₂O₈ (BAS) as an additive were synthesized by spark plasma sintering (SPS). The kinetic of densification, phase transformation sequences and grain growth during sintering process were investigated. Full densification could be achieved by 1600 °C without holding and using a heating rate of 100 °C min⁻¹, but the transformation from α-Si₃N₄ to α-SiAlON is not completed simultaneously with the densification process. The equilibrium phase assemblage could be reached after SPS at 1800 °C for 5 min and the resultant material possesses self-reinforced microstructure with high hardness of 19.2 GPa and fracture toughness of 6.8 MPa m^1/2. The complete crystallization of BAS is beneficial to the high temperature mechanical properties. The obtained could maintain the room strength up to 1300 °C.     

Stability and degradation of plasma deposited boron nitride thin films in ambient atmosphere

Boron nitride (BN) thin films were deposited at 296 K, 398 K, 523 K and 623 K by low power radio frequency plasma enhanced chemical vapor deposition with nitrogen (N₂) and hydrogen diluted diborane (15% B₂H₆ in H₂) source gases. Fourier transform infrared and UV–visible spectroscopies were used to investigate the stability and degradation of BN films under ambient air conditions. The action of moisture on the films is reduced with increasing substrate temperature (T_s) to the detriment of the film growth rate. This has been interpreted as related to the decrease in porosity and relative volume fraction of B–O containing disordered tissue at higher T_s. The thickness of the unstable films increases logarithmically with the air exposure time. Parallel to this, although the E₀₄ gap increases logarithmically with time, the Tauc gap remains the same. The increase of subgap absorptions and the decrease of Tauc slope with time indicate reduction of structural order. Crystallites of ammonium borate hydrates, the main product of the chemical reactions, are initially formed within the bulk. At a later time, as a result of increased porosity and disorder, the film thickness decreases while the islands of micro-crystallites rapidly grow above the surface of the film. Stability dependence on other deposition parameters was also studied: it is found that the 1260/1360 cm⁻¹ (O–B–O/B–N) infrared peak area ratio plays an indicator role to reveal the stability of BN films.     

Chemical deposition of Al2O3 thin films on Si substrates

Uniform Al₂O₃ films were deposited on silicon substrates by the sol–gel process from stable coating solutions. The technological procedure includes spin coating deposition and investigating the influence of the annealing temperature on the dielectric properties. The layers were studied by Fourier transform infrared spectroscopy and Scanning Electron Spectroscopy. The electrical measurements have been carried out on metal–insulator–semiconductor (MIS) structures. The C–V curves show a negative fixed charge at the interface and density of the interface state, Dit, 3.7 × 10¹¹ eV^− 1cm^− 2 for annealing temperature at 750 °C.     

Low-temperature fabrication of 0.65 PMN–0.35 PT by a mixed oxide method

Single-phase perovskite 0.65 PMN–0.35 PT was achieved at low temperature by a conventional mixed oxide method. It was prepared by ball-milling a mixture of PbO(orthorhombic), TiO₂, Nb₂O₅ and (MgCO₃)₄Mg(OH)₂·5H₂O instead of MgO and heat treatment at 800 °C for 2 h. The formation was studied by means of DSC, FT-IR, Coupled TG-Mass, XRD, and SEM. It proceeded via formation of PbO(tetragonal) and Pb₂Nb₂O₇(P₂N) intermediates to form perovskite phase. The pure perovskite PMN-PT powder was obtained in particle size of 0.5–0.8 μm, agglomerate-free, and pseudo-cube. The powder calcined at 600 °C was sintered to 97% T.D. at 900–1000 °C for 2 h and showed room temperature dielectric constant of 3200, loss of 1–2%, and specific resistance of 5 × 10¹¹ Ω cm.     

Bulk preparation and characterization of mesoporous carbon nanotubes by catalytic decomposition of cyclohexane on sol–gel prepared Ni–Mo–Mg oxide catalyst

Multiwalled carbon nanotubes were synthesized using Ni–Mo–Mg oxide catalyst prepared by sol–gel technique. Carbon nanotubes were formed in situ by the reduction of nickel oxide (NiO) and molybdenum oxide (MoO₃) to Ni and Mo by a gas mixture of nitrogen, hydrogen and cyclohexane at 750 °C. Scanning Electron Microscopy (SEM) was used to confirm the formation of carbon nanotubes (CNTs). The pore size distribution of carbon nanotubes (CNTs) was investigated by N₂ adsorption and desorption. It was found that the pore size fell into the mesopore range: 2 < d < 50 nm. Interpretation was also made using Raman spectroscopy, Diffuse reflectance spectroscopy, X-ray diffraction and ESR spectra. This method is found to produce a very high yield weighing over 20 times of the catalyst. Based on the experimental conditions and results obtained a possible growth mechanism of the carbon nanotubes is proposed.     

Barrier capability of Zr–N films with titanium addition against copper diffusion

Zr–Ti–N film prepared by sputtering deposition has been employed as a potential diffusion barrier for Cu metallization. It is thought that the existing states of Ti and Zr in the films are Ti–N and Zr–N phase in Zr–Ti–N films. Material analysis by XRD, XPS and sheet resistance measurement reveal that the failure of Zr–N film is mainly due to the formation of Cu₃Si precipitates at the Zr–N/Si interface by Cu diffusion through the grain boundaries or local defects of the Zr–N barrier layer into Si substrate. In conjunction with sheet resistance measurement, XRD and XPS analyses, the Cu/Zr–Ti–N/Si contact system has high thermal stability at least up to 700 °C. The incorporation of Ti atoms into Zr–N barrier layer was shown to be beneficial in improving the thermal stability of the Cu/barrier/Si contact system.     

Interface interaction in the B4C/(Fe–B–C) system

The wetting behavior in the B₄C/(Fe–C–B) system was investigated in order to clarify the role of Fe additions on the sinterability of B₄C. Iron and its alloys with C and B react with the boron carbide substrate and form a reaction zone consisting of a fine mixture of FeB and graphite. The apparent contact angles are relatively low for the alloys with a moderate concentration of the boron and carbon and allow liquid phase sintering to occur in the B₄C–Fe mixtures. A dilatometric study of the sintering kinetics confirms that liquid phase sintering actually takes place and leads to improved mass transfer. A thermodynamic analysis of the ternary Fe–B–C system allows accounting for the experimental observations.     

New powellite type oxides in Ca–R–Nb–Mo–O system (R = Y, La, Nd, Sm or Bi)—Their synthesis, structure and dielectric properties

New complex oxides having powellite (CaMoO₄) type structure in the Ca–R–Nb–Mo–O system (R = Y, La, Nd, Sm or Bi) were prepared employing the method of solid state reaction between the component oxides at high temperature (1000–1100 °C). The new compounds, CaRNbMoO₈ (R = Y, La, Nd, Sm, Bi) are colorless and electrical insulators. The dielectric constants (K at 1 MHz) of these compounds are in the range 14–33 and K shows very little variation in the temperature range 30–100 °C. Their temperature coefficient of dielectric constant (TCK) is negative, which varies from − 21 to − 220 ppm/°C.     

Effect of carbon content on the microstructure and properties of W–Si–C–N coatings fabricated by magnetron sputtering

A series of W–Si–C (4–5 at.%)–N nanocomposite coatings with different C contents have been deposited on Si wafer substrates by reactive magnetron sputtering of W–Si–C composite target in Ar + N₂ mixed atmosphere. Microstructure characteristics and mechanical properties of W–Si–C–N coatings were investigated in this paper. Results exhibited that W–Si–C–N coatings possess nanocomposite microstructure where nano-crystallites W₂(C, N) embedded in amorphous matrix of Si₃N₄/CNx/C. As the C content increased, the hardness and Youngs’ modulus of the W–Si–C–N coatings first increased and then decreased, reaching the maximum value of approximate 36 GPa and 382 GPa, respectively, for coatings containing 11.1 at.% C. All the coatings are in compressive stress state, ranging from 0.8 to 2.0 GPa. In addition, friction coefficient of the W–Si–C–N coatings considerably decreased with the increase of C content.     

Microstructure and mechanical properties of Al–20Si–5Fe–2X (X = Cu, Ni, Cr) alloys produced by melt-spinning

Al–20Si–5Fe–2X (X = Cu, Ni and Cr) ribbons were produced by melt-spinning and consolidated by hot pressing at 400 °C for 60 min. The microstructure of the ribbons and the consolidated alloys was investigated using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffractometry (XRD) method, and transmission electron microscopy (TEM). The hardness and compressive strength of the specimens at ambient and elevated temperatures were examined. The microstructure of the ribbons exhibited featureless and dendritic zones. Results of XRD and TEM showed formation of spherically shaped Si particles with an average diameter of 20 nm. Ultrafine Si (110–150 nm) and iron-containing intermetallic particles were noticed in the microstructure of the consolidated ribbons. An improved strength was achieved by alloying of Al–20Si–5Fe with Cu, Ni, and Cr. Nickel was found to be the most effective element in increasing the maximum stress, particularly at elevated temperatures.