Nanomechanical properties of FePtPd ternary alloy thin films

Presented in this study are crystalline structure and mechanical properties of FePt_0.75Pd_0.25 ternary alloy thin films deposited under the various annealing temperatures, obtained by means of transmission electron microscopy (TEM) and nanoindentation techniques. FePtPd ternary alloy thin films are deposited on Si substrates using a multi-target DC magnetron sputtering system. Results indicate that the grain size increase from 40 to 135 nm as the annealing temperature increases from 400 to 600 °C. From nanoindentation measurements, the hardness of FePtPd ternary alloy thin films are 11.6 ± 0.4, 10.4 ± 0.1 and 8.8 ± 0.3 GPa for the annealed temperatures of 400, 500 and 600 °C, respectively. And, the corresponding Young's moduli are 175.4, 152.2 and 142.6 GPa, respectively. Hardness for FePtPd ternary alloy thin films decreased slightly in accordance with the increase of the grain size. By fitting experimental results with the Hall-Petch equation, a probable lattice friction stress of 5.15 ± 0.05 GPa and Hall-Petch constant of 44.25 ± 2.55 GPa nm^1/2 are obtained.     

Synthesis of nano-TiC powder using titanium gel precursor and carbon particles

The paper presents a novel process for synthesis of nano-size titanium carbide by reaction between titanium bearing precursor gel and nano carbon particles derived from soot at different temperatures in the range of 1300-1580 °C for 2 h under argon cover. The HRTEM studies of TiC powder synthesized by heating at 1580 °C show the presence of cube shaped particles (~ 60-140 nm) and hollow rods (diameter ~ 30-185 nm). The average particle size of crystallites, calculated by Scherer equation is observed to be ~ 35 nm while the surface area-density measurements indicate it to be ~ 113 nm. The surface area decreases with increase in reaction temperature.     

Study on physical properties of indium-doped zinc oxide deposited by spray pyrolysis technique

Transparent conducting indium doped zinc oxide (IZO) thin films have been deposited on soda-lime glass substrates by the spray pyrolysis technique. The structural, electrical, and optical properties of these films were investigated as a function of substrate temperature. In this work the substrate temperature was varied between 350 °C and 500 °C. X-ray diffraction pattern reveals that at 350 °C dominant peak is (100) orientation. By increasing substrate temperature from 350 °C to 450 °C, sheet resistance decreases, from 302 Ω/□ to 26 Ω/□, then at 500 °C increases to 34 Ω/□. In the useful range for deposition (i.e. 450 °C to 500 °C), the orientation of the films was predominantly (002). The lowest sheet resistance (26Ω/□) is obtained at substrate temperature of about 450 °C with the transmittance of about 75%. Study of scanning electron microscopy images shows that films deposited at 400 °C, have grain size as large as 574 nm, while with increasing substrate temperature to 450 °C, grain size becomes smaller and reaches to a value of about 100 nm with spherical shape. At 500 °C grain size value would be around 70 nm with the same spherical shape.     

Effect of SPD and friction stir welding on microstructure and mechanical properties of Al-Cu-Mg-Ag sheets

Ultrafine grained (UFG) structure with an average grain size of ~ 0.6 μm was produced in sheets of Al-Cu-Mg-Ag alloy by equal channel angular pressing (ECAP) followed by hot rolling (HR) at 250 °C. These sheets were joined by friction stir welding (FSW) with efficiency of about unity. The effect of severe plastic deformation (SPD), FSW and heat treatment on the microstructure and mechanical properties of the welds and sheets was examined.     

Ethylene glycol assisted hydrothermal synthesis of flower like ZnO architectures

We describe a simple route to flower like ZnO architectures, based on the decomposition of zinc acetate precursor in water-ethylene glycol solution at 140-160 °C for 1d through hydrothermal method. The PXRD pattern reveals that the ZnO crystals are of hexagonal wurtzite structure. Ethylene glycol plays a key role on the morphology control of ZnO crystals. The SEM images of ZnO products prepared at 140 °C and 160 °C mainly exhibit flower like architecture composed of many rods. Whereas, the product prepared at 180 °C shows bunches accompanying a few number of free rods. TEM results reveal that the rods resemble swords with decrease in size from one end to another. From Raman spectrum, the peaks at 437 cm^− 1, 382 cm^− 1 and 411 cm^− 1 correspond to E₂ (high), A₁ (TO) and E₁ (TO) of ZnO crystals respectively. The photoluminescence spectrum exhibits strong UV emission at ~ 397 nm, which comes from recombination of exciton. The possible mechanism for the formation of flower like ZnO architecture is proposed.     

Preparation of high quality spray-deposited fluorine-doped tin oxide thin films using dilute di(n-butyl)tin(iv) diacetate precursor solutions

Fluorine-doped tin oxide (FTO) thin films were prepared, at different substrate temperatures, using dilute precursor solutions of di(n-butyl)tin(iv) diacetate (0.1 M DBTDA) by varying the F⁻ concentration in the solution. It is noticed that conductivity of FTO film is increasing by increasing the fluorine amount in the solution. Morphology of SEM image reveals that grain size and its distribution are totally affected by the substrate temperature in which conductivity is altered. Among these FTO films, the best film obtained gives an electronic conductivity of 31.85 × 10² Ω^− 1 cm^− 1, sheet resistance of 4.4 Ω/□ (ρ = 3.14 × 10^− 4 Ω cm) with over 80% average normal transmittance between the 400 and 800 nm wavelength range. The best FTO film consists of a large distribution of grain sizes from 50 nm to 400 nm range and the optimum conditions used are 0.1 M DBTDA, 0.3 M ammonium fluoride, in a mixture of propan-2-ol and water, at 470 °C substrate temperature. The large distribution of grain sizes can be easily obtained using low DBTDA concentration (~ 0.1 M or less) and moderate substrate temperature (470 °C).     

Hydrogen gas-sensing with bilayer structures of WO3 and Pd in SAW and electric systems

A bi-layer sensor structure of WO₃ (~ 100 nm) with a very thin film of palladium (Pd~ 18 nm) on the top, has been studied for hydrogen gas-sensing application at ~ 80 °C and ~ 120 °C and low hydrogen concentrations (0.025-1%). The structures were obtained by vacuum deposition (first the WO₃ and then the Pd film) onto a LiNbO₃ Y-cut Z-propagating substrate making use of the Surface Acoustic Wave method and additionally (in this same technological processes) onto a glass substrate with a planar microelectrode array for simultaneous monitoring of planar resistance of the structure. A very good correlation has been observed between these two methods — frequency changes in SAW method correlate very well with decreases in the bi-layer structure resistance. The SAW method is faster at the lower interaction temperature such as 80 °C, whereas at an elevated temperature of 120 °C, the electrical planar method is also fast and has a lower limit of detection.     

Dependence of carrier lifetime on Cu-contacting temperature and ZnTe:Cu thickness in CdS/CdTe thin film solar cells

Cu diffusion from a ZnTe:Cu contact interface can increase the net acceptor concentration in the CdTe layer of a CdS/CdTe photovoltaic solar cell. This reduces the space-charge width (W_d) of the junction and enhances current collection and open-circuit voltage. Here we study the effect of Cu concentration in the CdTe layer on carrier lifetime (τ) using time-resolved photoluminescence measurements of ZnTe:Cu/Ti-contacted CdTe devices. Measurements show that if the ZnTe:Cu layer thickness remains constant and contact temperature is varied, τ increases significantly above its as-deposited value when the contacting temperature is in a range that has been shown to yield high-performance devices (~ 280° to ~ 320 °C). However, when the contacting temperature is maintained near an optimum value and the ZnTe:Cu thickness is varied, τ decreases with ZnTe:Cu thickness.     

Structural and electrical properties of BiFeO3 thin films by solution deposition and microwave annealing

Lead-free polycrystalline BiFeO₃ (BFO) thin films were developed using a chemical solution deposition method to deposit the films and the multi-mode 2.45 GHz microwave furnace to optimize the annealing condition of the films. Phase-pure BFO films were obtained at 500 °C-600 °C for 1-5 min with a heating rate of 10 °C/min. The film by microwave annealing (MW) at 550 °C for 5 min exhibited a (012)-preferred orientation with a dense morphology of grain size ~ 294 nm. Its dielectric constant of 96.2, low leakage current density of 2.466 × 10^− 6 A/cm², polarization (2P_r) and coercive field (2E_c) of 0.931 μC/cm² and 57.37 kV/cm, respectively, were improved compared to those by conventional annealing (CA) at the same annealing conditions.     

Grain size dependence of pure β-eucryptite thermal expansion coefficient

The impact of the grain size, in the range of about ~ 3-12 μm, on spontaneous microcracking and therefore on the value of the bulk β-eucryptite negative thermal expansion coefficient (TEC) has been carefully investigated. In order to control the grain size, pure β-eucryptite powders were synthesized, slip-casted and sintered in air at 1300 °C for 0, 6 and 24 h. The results show that only a slight variation of the intrinsic β-eucryptite TEC is obtained after sintering. On the contrary, the larger the grain size the more important the microcracking phenomenon, leading to a significant and progressive decrease of the bulk β-eucryptite TEC.     

The effects of substrate temperature on the structure and properties of ZnO films prepared by pulsed laser deposition

ZnO thin films were prepared by pulsed laser deposition (PLD) on glass substrates with growth temperature from room temperature (RT) to 500 °C. The effects of substrate temperature on the structural and optical properties of ZnO films have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission spectra, and RT photoluminescence (PL) measurements. The results showed that crystalline and (0 0 2)-oriented ZnO films were obtained at all substrate temperatures. As the substrate temperature increased from RT to 500 °C, the ratio of grain size in height direction to that in the lateral direction gradually decreased. The same grain size in two directions was obtained at 200 °C, and the size was smallest in all samples, which may result in maximum E_g and E₀ of the films. UV emission was observed only in the films grown at 200 °C, which is probably because the stoichiometry of ZnO films was improved at a suitable substrate temperature. It was suggested that the UV emission might be related to the stoichiometry in the ZnO film rather than the grain size of the thin film.     

Combined hardening and non-hardening embrittlement of an interstitial free steel

The ductile-to-brittle transition temperature (DBTT) and hardness of an interstitial free steel solid-solution-strengthened by phosphorus are experimentally evaluated under different conditions. The results demonstrate a linear relationship between DBTT and hardness under constant phosphorus grain boundary concentration and grain size. The DBTT increases with increasing hardness, showing a hardening embrittlement effect. With reference to a previous study concerning the effect of phosphorus boundary segregation on the ductile-to-brittle transition for the same steel, which shows a non-hardening embrittlement effect, it is seen that the two embrittlement effects are independent of each other and that the combined embrittlement effect under an average grain size of ~ 70 μm can be expressed as DBTT (°C) = 0.24H_V + 1.60C_P − 34.8, where H_V is the Vickers hardness value and C_P is the phosphorus boundary concentration in at.%.     

New dielectric material system of x(Mg0.95Zn0.05Ti)O3-(1 − x)Ca0.8Sm0.4/3TiO3 at microwave frequency

The microstructures and the microwave dielectric properties of the x(Mg_0.95Zn_0.05)TiO₃-(1 − x) Ca_0.8Sm_0.4/3TiO₃ ceramic system were investigated. In order to achieve a temperature-stable material, we studied a method of combining a positive temperature coefficient material with a negative one. Ca_0.8Sm_0.4/3TiO₃ has dielectric properties of dielectric constant ε_r ~ 120, Q × f value ~ 13,800 GHz and a large positive τ_f value ~ 400 ppm/°C. (Mg_0.95Zn_0.05)TiO₃ possesses high dielectric constant (ε_r ~ 16.21), high quality factor (Q × f value ~ 210,000 at 9 GHz) and negative τ_f value (− 59 ppm/°C). Sintering at 1300 °C with x = 0.9, 0.9(Mg_0.95Zn_0.05Ti)O₃ − 0.1 Ca_0.8Sm_0.4/3TiO₃ has a dielectric constant (ε_r) of 22.7, a Q × f value of 124,000 GHz and a temperature coefficient of resonant frequency (τ_f) of − 6.3 ppm/°C.     

Temperature dependent microstructure of MTES modified hydrophobic silica aerogels

Hydrophobic silica aerogels were prepared using a single step sol-gel process followed by ethanol supercritical drying. Using tetraethoxysilane (TEOS) as a precursor and ammonium hydroxide as a catalyst the aerogel surface was chemically modified with methyltriethoxysilane (MTES). A MTES/TEOS molar ratio of 0.5 (M5) was used. The microstructure of the surface modified aerogels was evaluated as a function of heat treatment temperature over a range of 200-500 °C. The thermal stability was analyzed by simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC) and the microstructure was evaluated by physisorption analysis (BET) and scanning electron microscopy (SEM). The chemical composition and hydrophobicity/hydrophilicity of the aerogels were investigated by Fourier Transform-Infrared (FT-IR) spectroscopy. The M5 aerogels, which were initially hydrophobic, exhibited partial hydrophilicity at treatments above 244.5 °C and complete hydrophilicity above 429.9 °C. The surface area of the aerogels ranged from 776.65-850.20 m²/g. Pore size increased after heat treatment, ranging from 16.25 to 18.52 nm vs. an initial pore size of 14.71 nm. The maximum pore size of 18.52 nm was found at the lowest heat treatment temperature (~ 200 °C). Heat treatment had a mixed effect on the pore volume, as pore volumes decreased at lower treatments (~ 200-400 °C) and increased at higher heat treatments (~ 450-500 °C) relative to the untreated aerogels. With initial heat treatment the Si-CH₃ group began to oxidize to Si-OH. Aerogels heated above 429.9 °C exhibited hydroxyl polymerization leading to aerogels with large particles and a dense microstructure.     

Microstructural response on the cracking resistance of alloy 600

Precipitation of chromium rich carbides promotes the development of a Cr-depleted zone which in turn provided a weak path for the intergranular crack propagation. The role of low temperature anneals on the intergranular cracking resistance (IGC) of alloy 600 was investigated using modified wedge opening loading specimens heat treated at 930, 800 and 600 °C and exposed to high purity water pressurized with hydrogen at 300 °C. Mill annealing at 930 °C did lead to IGC susceptible microstructures. In this condition the alloy 600 exhibited the least crack growth rates (da / dt) of the order of 1.86 × 10^− 12 m/s and characterized the substantial work hardening ahead of the crack front. In contrast, annealing at 600 °C (HT600) resulted in increasing IGC susceptibilities. Under these conditions, crack growth rates, da / dt, as high as 7.10 × 10^− 10 m/s were found (HT600). Accordingly, significant interactions between the slip bands and the crack path lead to crack bifurcation into the slip planes and cavity formation.     

High temperature deformation of titanium diboride

Specimens of high purity polycrystalline titanium diboride, TiB₂, were tested in uniaxial compression under vacuum at a strain rate of 5 × 1O^–4sec^–1 to determine the plastic yield behaviour. Generally, plastic deformation was detected only above 170O° C. The apparatus was able to apply u stress of 900 MPa at a maximum temperature of 2000° C. The yield stress data fit an Arrhenius function, with an apparent activation energy of O.8 eV atom^–1. Dislocation glide over the Peierls barrier is thought to be the deformation mechanism, The dependence of the yield stress on the grain size obeyed the Hall-Petch relation within the bounds of experimental error. A TiB₂ single crystal containing TiC precipitates was also compression - tested at 2000° C, and its yield stress was approximately four times the stress predicted by the Hall-Petch expression for e pure TiB₂ single crystal, suggesting that the precipitate raises the yield stress but that the intrinsic lattice resistance is still significant. Submicrometre-sized graphite inclusions were observed in the polycrystalline specimens, but are thought not to have a direct effect on the yield stress in the temperature regime of the present study.     

Deposition of silicon nitride thin films by hot-wire CVD at 100 °C and 250 °C

Silicon nitride thin films for use as passivation layers in solar cells and organic electronics or as gate dielectrics in thin-film transistors were deposited by the Hot-wire chemical vapor deposition technique at a high deposition rate (1-3 ?/s) and at low substrate temperature. Films were deposited using NH₃/SiH₄ flow rate ratios between 1 and 70 and substrate temperatures of 100 °C and 250 °C. For NH₃/SiH₄ ratios between 40 and 70, highly transparent (T ~ 90%), dense films (2.56-2.74 g/cm³) with good dielectric properties and refractive index between 1.93 and 2.08 were deposited on glass substrates. Etch rates in BHF of 2.7 ?/s and < 0.5 ?/s were obtained for films deposited at 100 °C and 250 °C, respectively. Films deposited at both substrate temperatures showed electrical conductivity ~ 10^− 14 Ω^− 1 cm^− 1 and breakdown fields > 10 MV cm^− 1.     

Low resistivity metal lines formed by functional liquids and successive treatment of catalytically generated hydrogen atoms in the Cat-CVD system

Metal-interconnection among electrodes is an important process to fabricate electronic devices. A novel high-speed technique using silver (Ag) functional liquid to form Ag lines is proposed. For improvement of the electrical conductivity of the Ag lines, atomic hydrogen (H) generated by the Cat-CVD system is used. There is a sintering phenomenon among Ag nanoparticles (~ 50 nm) during H treatment at low substrate temperatures (~ 100 °C). Scanning electron microscopy (SEM) reveals that the Ag grain size increases with H annealing duration, which results in the resistivity of the Ag lines on an order of 10⁻⁶ Ω cm.     

Plastic behaviour of CuAl2

The plastic behaviour of CuAl₂ was studied by compression testing of single crystals and polycrystals in the temperature range 300–575 °C. While single crystals were grown from the melt by the Bridgeman technique, ingot and powder metallurgy routes were adopted for polycrystalline specimens. In addition to exploring their flow behaviour, the deformation mechanism was assessed through thermal activation analysis. It was observed that CuAl₂ failed in a brittle manner in compression below 375 °C and its ductility improved progressively with temperature. The brittle-ductile transition (BDT) temperature was influenced by the initial dislocation density but not by the grain size. The strong temperature dependence of flow stress and grain size strengthening effect as per the Hall-Petch relation, were dominant up to nearly the melting temperature of CuAl₂. The measured activation parameters for deformation suggest that the Peierls mechanism is rate controlling over the investigated temperature range.     

Rapid synthesis of ZnO ellipsoidal nanostructures in large scale and their photoluminescence properties

ZnO ellipsoidal nanostructures with uniform ellipsoidal morphologies have been synthesized using different hydroxide anion precursors by an ultra-fast, facile (90 °C) solution-phase method without the assistance of sonication or any surfactants. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence (PL) measurements. Based on the experimental results, a growth mechanism of ZnO nanostructures was proposed. The obtained ZnO nanostructures exhibit a weak UV emission band at ~ 385 nm and a relatively stronger orange emission band at ~ 615 nm. The solution-phase method is simple, convenient for large-scale fabrication of ZnO ellipsoidal nanostructures.