Synthesis and phases evolution of Si–C–Ti from polycarbosilane (PCS) and metal Ti

Si–C–Ti ceramics were synthesized by reactive pyrolysis of polycarbosilane (PCS) precursor filled with metal Ti powder. Pyrolysis of mixture with atomic ratio of Ti:Si through 3:1–3:2 was carried out in argon atmosphere at given temperature up to 1500 °C. The metal–precursor reactions, and phase evolution were studied using X-ray diffraction and scanning electron microscopy with EDX. The Ti₃SiC₂ phase was obtained firstly from reaction of PCS and Ti. Ti₃SiC₂ formation starts at 1300 °C and its amount increases significantly in a narrow temperature range between 1400 °C and 1500 °C. In addition, addition of CaF₂ can promote the formation of Ti₃SiC₂ phase.     

Structural and chemical characterization of precipitates in Al-2024/TiC composites

Structural characterizations based on transmission electron microscopy observations were carried out on as-fabricated and heat-treated Al-2024/TiC composites. These composites types reinforced with TiC particles were produced with a pressureless melt infiltration route at 1200 °C for 2 h under argon atmosphere. The composites were heat-treated at 530 °C during 150 min, cold-water quenched and subsequently artificial and natural aged at 190 °C for 12 h in an argon environment and at room temperature for 96 h, respectively. Different precipitate types were obtained and they were identified as CuAl₂, Al₃Ti, Ti₃AlC and Ti₃Al. Most of the precipitates were found to be uniformly distributed in the matrix and some regions show precipitates which have a cubic morphology (Ti₃Cu). High-resolution electron microscopy images were partially used for the characterization of the precipitates in these composites.     

Dependence of dynamic strain ageing on strain amplitudes during the low-cycle fatigue of TP347H austenitic stainless steel at 550 °C

Low-cycle fatigue (LCF) tests are carried out on TP347H stainless steel at a strain rate of 8 × 10⁻³ s⁻¹ with total strain amplitudes (Δε_t/2) of ±0.4% and ±1.0%, at room temperature (RT) and 550 °C. It is found that the stress responses and dislocation structures under cyclic loading strongly depend on the value of strain amplitude at 550 °C. Compared with those at the same strain amplitude at RT, the material shows a rapid strain softening, and finally attains a stabilized state at Δε_t/2 = ±0.4% and 550 °C, but the one presents an anomalous behavior, i.e., first a rapid hardening to the maximum stress, followed by a reducing softening at Δε_t/2 = ±1.0% and 550 °C. More cells resulting from dislocation cross-slip and planar structures due to dynamic strain ageing (DSA) restricting cross-slip develop at low strain amplitude of ±0.4% at the first cycle. However, there are more complicated dislocation structures, such as cells, elongated cells, walls/channels and planar structures at Δε_t/2 = ±1.0%. The observations of scanning electron microscopy (SEM) and transmission electron microscopy (TEM) exclude the effects of martensitic transformation, creep, oxidation, and precipitations on these stress responses and microstructure evolutions, which result from DSA appearing at 550 °C.     

Oxidation behavior of amorphous metallic Ni3(SbTe3)2 compound

Amorphous Ni₃(SbTe₃)₂ compound was prepared from a metathesis between Zintl phase K₃SbTe₃ and NiBr₂ in solution and its oxidation behavior was investigated in the temperature range of 200–700 °C in air. To characterize the sample, thermogravimetry (TG), X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive analysis by X-ray (EDAX) analyses were performed and electrical conductivity was measured as a function of temperature in the range of 25–800 °C in air. The specimen showed a metallic conducting-like behavior below 585 °C while a semiconducting-like behavior above 585 °C. At a first oxidation step of Ni₃(SbTe₃)₂ below 500 °C, TeO₂ phase is formed. Above 500 °C, NiO phase is formed, then some NiO reacts with TeO₂ to form NiTeO₃ and NiSb₂O₆ is simultaneously formed. Above 700 °C, NiTeO₃ is further reacted with TeO₂ to form NiTe₂O₅. Both NiTeO₃ and NiTe₂O₅ are decomposed above 774 °C.     

Diffusion bonding of titanium alloy to micro-duplex stainless steel using a nickel alloy interlayer: Interface microstructure and strength properties

In the present study, diffusion bonding of titanium alloy and micro-duplex stainless steel with a nickel alloy interlayer was carried out in the temperature range of 800–950 °C for 45 min under the compressive stress of 4 MPa in a vacuum. The bond interfaces were characterised by scanning electron microscopy, electron probe microanalyzer and X-ray diffraction analysis. The layer wise Ni₃Ti, NiTi and NiTi₂ intermetallics were observed at the nickel alloy/titanium alloy interface and irregular shaped particles of Fe₂₂Mo₂₀Ni₄₅Ti₁₃ was observed in the Ni₃Ti intermetallic layer. At 950 °C processing temperature, black island of β-Ti phase has been observed in the NiTi₂ intermetallics. However, the stainless steel/nickel alloy interface indicates the free of intermetallics phase. Fracture surface observed that, failure takes place through the NiTi₂ phase at the NiA–TiA interface when bonding was processed up to 900 °C, however, failure takes place through NiTi₂ and β-Ti phase mixture for the diffusion joints processed at 950 °C. Joint strength was evaluated and maximum tensile strength of ∼560 MPa and shear strength of ∼415 MPa along with ∼8.3% ductility were obtained for the diffusion couple processed at 900 °C for 45 min.     

The study of tribological and corrosion behavior of plasma nitrided 34CrNiMo6 steel under hot and cold wall conditions

This paper reports on a comparative study of tribological and corrosion behavior of plasma nitrided 34CrNiMo6 low alloy steel under modern hot wall condition and conventional cold wall condition. Plasma nitriding was carried out at 500 °C and 550 °C with a 25% N₂ + 75% H₂ gas mixture for 8 h. The wall temperature of the chamber in hot wall condition was set to 400 °C. The treated specimens were characterized by using scanning electron microscopy (SEM), X-ray diffraction (XRD), microhardness and surface roughness techniques. The wear test was performed by pin-on-disc method. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) tests were also used to evaluate the corrosion resistance of the samples. The results demonstrated that in both nitriding conditions, wear and corrosion resistance of the treated samples decrease with increasing temperature from 500 °C to 550 °C. Moreover, nitriding under hot wall condition at the same temperature provided slightly better tribological and corrosion behavior in comparison with cold wall condition. In consequence, the lowest friction coefficient, and highest wear and corrosion resistance were found on the sample treated under hot wall condition at 500 °C, which had the maximum surface hardness and ε-Fe_2–3N phase.     

Alumina–tantalum composite for femoral head applications in total hip arthroplasty

Dense composite laminates of alumina (Al₂O₃) and tantalum (Ta) were fabricated by hot pressing and tested in vitro for potential use as a femoral head material in total hip arthroplasty (THA). Al₂O₃–Ta composite laminates hot pressed at 1450 °C and 1650 °C had flexural strengths of 940 ± 180 MPa and 1090 ± 340 MPa, respectively, which were far larger than the values of 420 ± 140 MPa and 400 ± 130 MPa for Al₂O₃ hot pressed at 1450 °C and 1650 °C, respectively. The interfacial shear strength, determined by a double-notched specimen test, was 310 ± 80 MPa for the composite laminate hot pressed at 1650 °C, indicating strong interfacial bonding between Al₂O₃ and Ta. Scanning electron microscopy (SEM), energy dispersive X-ray (EDS) analysis, and X-ray mapping of polished sections of the hot-pressed laminates showed the presence of an interfacial region formed presumably by diffusion of O (at 1450 °C) or O and Al (1650 °C) from Al₂O₃ into Ta. Composite femoral heads of Al₂O₃ and Ta could combine the low wear of an Al₂O₃ articulating surface with the safety of a ductile metal femoral head.     

The L12 CrPt3 underlayer effect on the ordering of L10 FePt films

This study discusses the effects of a CrPt₃ alloy underlayer on the magnetic properties and microstructure of FePt films. The L1₂ CrPt₃ phase was chemical long-range ordered at a temperature above 600 °C, and the 120-nm thick CrPt₃ film annealed at 800 °C, resulting in ferrimagnetic behavior. The long-range ordered CrPt₃ underlayer slightly increased the ordering of the L1₀ FePt film, as evidenced by the individual L1₂ CrPt₃ and L1₀ FePt (0 0 1) superlattice peaks. An X-ray slow scan of the [FePt/CrPt₃(T °C)]_400°C bilayer shows that the integrated intensity of the L1₀ FePt (0 0 1) peaks was higher on the long-range order L1₂-type CrPt₃ (T = 600, 800) underlayer and lower on the partial short-range order L1₂ and A₁-types CrPt₃ (T = 400) underlayer. However, optimal magnetic properties were obtained in the [FePt/CrPt₃(400 °C)]_400°C bilayer. When a FePt film is deposited on a ferrimagnetic CrPt₃(800 °C) underlayer, the resulting bilayer shows isotropic magnetic hysteresis loops and cannot be saturated at 1.8 T. Atomic force microscopy (AFM) and transition electron microscopy (TEM) show that the L1₂ CrPt₃(800 °C) underlayer exhibits coarse surface roughness and plate-like grains, respectively. From TEM images, all the FePt grains were isolated uniformly by CrPt₃ matrix.     

Characterization of domain configurations in LiTaO3/Al2O3 ceramic composites

Characterization of domain configurations in 15 vol% LiTaO₃/Al₂O₃ ceramic composites hot-pressed sintered at 1300 °C was carried out using transmission electron microscopy and high-resolution transmission electron microscopy. Mainly banded- and wedge-shaped 90° domains, with few 180° domains, were formed in the LiTaO₃ grains within the composite. The formation of 90° domains was attributed to the large stress caused by residual polarization. Many dark dots, distributed along the 90° domain boundaries, were detected and it was confirmed that they were not a deposited second phase but a type of contrast induced by high strain. The 90° domain boundaries presented an α-type fringe contrast and no δ-type fringes were observed, indicating that they were of the non-conventional type.     

Low temperature preparation and characterization of CdTiO3 nanoplates

An alternative low cost method was proposed for the low temperature (600 °C) preparation of CdTiO₃ nanoplates, using low-melting-point Cd(NO₃)₂ · 4H₂O and high-reactive-activity TiO₂ nanocrystals as the reactants. The structure, composition, specific surface area, thermal stability and optical properties of the as-synthesized products were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy, field emission scanning electron microscopy, Brunauer–Emmett–Teller surface area analysis, UV–vis absorption and room temperature photoluminescence spectra. The as-synthesized CdTiO₃ nanoplates were thermally stable at temperatures ≤ 900 °C, and their phase changed from ilmenite to perovskite when heated in air at 1000 °C for 2 h. Besides, they exhibited a strong and broad visible light emission in the range of about 470–750 nm upon laser excitation at 325 nm, enabling their use as a luminescent material.     

Al2TiO5–Al2O3–TiO2 nanocomposite: Structure,mechanical property and bioactivity studies

Novel biomaterials are of prime importance in tissue engineering. Here, we developed novel nanostructured Al₂TiO₅–Al₂O₃–TiO₂ composite as a biomaterial for bone repair. Initially, nanocrystalline Al₂O₃–TiO₂ composite powder was synthesized by a sol–gel process. The powder was cold compacted and sintered at 1300–1500 °C to develop nanostructured Al₂TiO₅–Al₂O₃–TiO₂ composite. Nano features were retained in the sintered structures while the grains showed irregular morphology. The grain-growth and microcracking were prominent at higher sintering temperatures. X-ray diffraction peak intensity of β-Al₂TiO₅ increased with increasing temperature. β-Al₂TiO₅ content increased from 91.67% at 1300 °C to 98.83% at 1500 °C, according to Rietveld refinement. The density of β-Al₂TiO₅ sintered at 1300 °C, 1400 °C and 1500 °C were computed to be 3.668 g cm^?3, 3.685 g cm^?3 and 3.664 g cm^?3, respectively.Nanocrystalline grains enhanced the flexural strength. The highest flexural strength of 43.2 MPa was achieved. Bioactivity and biomechanical properties were assessed in simulated body fluid. Electron microscopy confirmed the formation of apatite crystals on the surface of the nanocomposite. Spectroscopic analysis established the presence of Ca and P ions in the crystals. Results throw light on biocompatibility and bioactivity of β-Al₂TiO₅ phase, which has not been reported previously.     

Vapor phase growth of GaN crystals with different morphologies and orientations on graphite and sapphire substrates

GaN crystals were grown on graphite and sapphire substrates at 990–1050 °C by reaction of Ga₂O with flowing NH₃. Ga₂O gas was produced at a constant rate (1.3 wt% min⁻¹) by reaction of Ga₂O₃ with carbon at 1000–1060 °C. The effect of NH₃ concentration (3–100 vol%) and the nature of the substrate on the morphology and orientation of the GaN crystals were determined by scanning electron microscopy, transmission electron microscopy, X-ray diffraction and selected area electron diffraction. It was found that sheet and plate-like crystals grew at different orientations to the substrate with different NH₃ concentrations and substrates.     

Effect of reaction temperature on crystallite size and sensing response of chromium oxide nanoparticles

Nanoparticles of chromium oxide have been synthesized following a precipitation technique at reaction temperatures 5, 27 and 65 °C. Synthesized powders were characterized using X-ray diffraction, transmission electron microscope and Brunauer–Emmett–Teller techniques to carry out structural and morphological analysis. The reaction temperature has been found to be playing a crucial role in controlling particle size. It has been observed that Cr₂O₃ nanoparticles synthesized at 27 °C were smaller as compared to those synthesized at 5 and 65 °C. Chromium oxide samples thus prepared were deposited as thick films on alumina substrates to act as gas sensors and their sensing response to ethanol vapour was investigated at different operable temperatures. It has been observed that all the sensors exhibited optimum response at 250 °C. The investigations revealed that sensing response of Cr₂O₃ nanoparticles synthesized at 27 °C was exceptionally higher than that of Cr₂O₃ nanoparticles synthesized at 5 and 65 °C.     

Effects of heat treatment on the microstructure of amorphous boron carbide coating deposited on graphite substrates by chemical vapor deposition

A two-layer boron carbide coating is deposited on a graphite substrate by chemical vapor deposition from a CH₄/BCl₃/H₂ precursor mixture at a low temperature of 950 °C and a reduced pressure of 10 KPa. Coated substrates are annealed at 1600 °C, 1700 °C, 1800 °C, 1900 °C and 2000 °C in high purity argon for 2 h, respectively. Structural evolution of the coatings is explored by electron microscopy and spectroscopy. Results demonstrate that the as-deposited coating is composed of pyrolytic carbon and amorphous boron carbide. A composition gradient of B and C is induced in each deposition. After annealing, B₄C crystallites precipitate out of the amorphous boron carbide and grow to several hundreds nanometers by receiving B and C from boron-doped pyrolytic carbon. Energy-dispersive spectroscopy proves that the crystallization is controlled by element diffusion activated by high temperature annealing, after that a larger concentration gradient of B and C is induced in the coating. Quantified Raman spectrum identifies a graphitization enhancement of pyrolytic carbon. Transmission electron microscopy exhibits an epitaxial growth of B₄C at layer/layer interface of the annealed coatings. Mechanism concerning the structural evolution on the basis of the experimental results is proposed.     

Application of carbonated apatite coating on a Ti substrate by aqueous spray method

The fabrication and characterization of a carbonate-containing apatite film deposited on a Ti plate via an aqueous spray method is described. The mist of the spray solution emitted from a perpendicularly oriented airbrush was made to strike a warmed Ti substrate. The thicknesses of the sprayed film and those heat-treated at 400 °C–700 °C under Ar gas flow were in the range 1.21–1.40 μm. The results of elemental analyses and Fourier transform infrared spectroscopy of the powders that were mechanically collected from the surface of the sprayed film suggest that the film was Ca₁₀(PO₄)6(CO₃) · 2CO₂ · 3H₂O. The presence of the carbonate ion and the lattice CO₂ molecule was confirmed via the aforementioned analyses; the finding was also consistent with the X-ray diffraction patterns of the films and the chemical identity of the sprayed and heat-treated films that were measured using X-ray photoelectron spectroscopy. The sprayed film comprises a characteristic network structure, which contains round particles within the networks, as was observed by field-emission scanning electron microscopy. A scratch test indicated that the shear stress of the sprayed film (21 MPa) significantly improved to 40 and > 133 MPa after heat-treatment at 600 °C and 700 °C, respectively, under Ar gas flow for 10 min.     

The effect of fabrication processes on the mechanical and interfacial properties of SiCf/Cu–matrix composites

Three groups of SiC_f/Ti/Cu composites were prepared under conditions of 650 °C + 105 min (sample 1#), 750 °C + 85 min (sample 2#) and 840 °C + 50 min (sample 3#), respectively, by foil-fiber-foil method (FFF), and their room temperature tensile strengths were established. The aim is to model the reactive bonding states between Ti and SiC fiber and between Ti and Cu when Ti is used as interfacial adhesion promoters in SiC_f/Cu–matrix composites. The fracture surfaces, SiC_f/Ti interfaces and Ti/Cu interfaces were investigated by scanning electron microscopy (SEM), optical microscopy and energy dispersive spectroscopy (EDS). The tensile tests show that the tensile strengths of samples 1# and 2# are not obviously enhanced due to the weak bonding strength between SiC fiber and Ti, while those of sample 3# are achieved above 90% of ROM (the rule of mixtures) strength because of excellent bonding between SiC fiber and Ti. However, there are distinct Ti/Cu interfacial reaction zones after the three processes, which are approximately 5.4, 9.0 and 13.3 μm thick, respectively. The Ti/Cu interfacial reaction products are mainly distributed in four layers. In samples 1# and 2#, the products are predicted to be Cu₄Ti, Cu₃Ti₂, CuTi and CuTi₂ according to their chemical compositions determined by EDS, while in sample 3#, the products are Cu₄Ti, Cu₄Ti₃, CuTi and CuTi₂. Additionally, the relationships between the thickness of Ti interlayer and its reaction with C and Cu are also discussed, and an optimal thickness of Ti is introduced.     

Longitudinal and concurrent dimensional changes of cellulose aggregate fibrils during sorption stages

Atomic force microscopy (AFM) studies of the dimensional changes of cellulose microfibril materials, called cellulose aggregate fibrils (approx. 100 µm × 3 µm × 300 nm), exposed to two distinct relative humidities of 80% and 23% for 24 h and then suddenly subjected to 50% RH and 23 °C show that the fibrils are responsive to the surrounding environments in a nonspecific fashion. AFM images (10 µm × 10 µm) of the individual straight cellulose aggregate fibrils were taken as a function of elapsed time during both desorption and adsorption of moisture. The longitudinal distance between discrete natural defects observed on the cellulose aggregate fibrils as well as the width, cross-sectional area, and height of the cellulose aggregate fibril were measured from the AFM images. The length of the cellulose aggregate fibrils was found to have reduced after exposure to either high or low relative humidity, and then placement in ambient conditions. Over time in ambient conditions, the cellulose aggregate fibrils progressively relaxed to their original length during both desorption and adsorption of moisture. However, the relaxation rate during adsorption was faster than that during desorption. The possible explanations for this phenomenon are discussed including the sample preparation method, volume conservation, entropy elasticity, and free volume theory. The changes in the width, height, and cross-sectional area are also discussed.     

Effect of ZrO2-doping of nanosized Fe2O3/MgO system on its structural,surface and catalytic properties

Fe₂O₃/MgO system was prepared by wet impregnation method followed by treatment with different amounts of Zr-dopant salt then heating at 500 and 700 °C. The dopant concentrations were 0.48, 0.95 and 1.4 mol% ZrO₂. Pure and variously doped solids were characterized using XRD, N₂-adsorption isotherms carried out at ?196 °C and catalytic decomposition of H₂O₂ in aqueous solution at 25–35 °C. The results revealed that the nanosized MgO phase was only detected in the diffractograms of pure and doped solids calcined at 500 °C. Heating pure and doped solids at 700 °C produced nanosized MgFe₂O₄ phase together with MgO phase. Pure and ZrO₂-doped solids calcined at 500 and 700 °C are mesoporous adsorbents. The doping process brought about a measurable decrease in the S_BET of Fe₂O₃/MgO system with subsequent increase in its catalytic activity. The catalytic activity of the investigated system toward H₂O₂ decomposition, expressed as reaction rate constant per unit surface area was found to increase as a function of dopant concentration. The maximum increase in the reaction rate constant per unit surface area measured for the reaction carried out at 30 °C attained 125% for the heavily doped samples. This significant increase was based on the catalytic activity of pure catalyst sample measured under the same conditions.     

Friction force microscopy study of annealed diamond-like carbon film

In this paper we introduce mechanical and structural characteristics of diamond-like carbon (DLC) films which were prepared on silicon substrates by radio frequency (RF) plasma enhanced chemical vapor deposition (PECVD) method using methane (CH₄) and hydrogen (H₂) gas. The films were annealed at various temperatures ranging from 300 to 900 °C in steps of 200 °C using rapid thermal processor (RTP) in nitrogen ambient. Tribological properties of the DLC films were investigated by atomic force microscopy (AFM) in friction force microscopy (FFM) mode. The structural properties of the films were obtained by high resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The wettability of the films was obtained using contact angle measurement. XPS analysis showed that the sp³ content is decreased from 75.2% to 24.1% while the sp² content is increased from 24.8% to 75.9% when the temperature is changed from 300 to 900 °C. The contact angles of DLC films were higher than 70°. The FFM measurement results show that the highest friction coefficient value was achieved at 900 °C annealing temperature.     

Experimental study of diffusion welding/bonding of titanium to copper

In the present study, Ti–6Al–4V alloy was bonded to electrolytic copper at various temperatures of 875, 890 and 900 °C and times of 15, 30 and 60 min through diffusion bonding. 3 MPa uniaxial load was applied during the diffusion bonding. Interface quality of the joints was assessed by microhardness and shear testing. Also, the bonding interfaces were analysed by means of optical microscopy, scanning electron microscopy and energy dispersive spectrometer. The bonding of Ti–6Al–4V to Cu was successfully achieved by diffusion bonding method. The maximum shear strength was found to be 2171 N for the specimen bonded at 890 °C for 60 min. The maximum hardness values were obtained from the area next to the interface in titanium side of the joint. The hardness values were found to decrease with increasing distance from the interface in titanium side while it remained constant in copper side. It was seen that the diffusion transition zone near the interface consists of various phases of βCu₄Ti, Cu₂Ti, Cu₃Ti₂, Cu₄Ti₃ and CuTi.