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In this research, the effect of milling time and annealing temperature on a heat activated synthesis of barium hexaferrite from mechanically activated mixture of hematite and barium acetate was investigated. The properties of samples were examined by XRD, DTA/TGA, SEM and VSM methods. The initial mixture with Fe/Ba molar ratio of 11 was milled for 24–48 h and then annealed at 800–1100°C. The XRD results showed the reflections of hematite as a major phase and barium hydroxide as a minor phase during mechanical milling in all three samples. It was observed that the specimen milled for 48 h exhibits the smallest mean crystallite size of 25 nm for hematite, as major phase. XRD results showed that annealing at 1100°C produces more pure barium hexaferrite phase comparing to lower temperatures. So, it was concluded that single phase BaFe₁₂O₁₉ can be achieved by milling for 48 h and then annealing at 1100°C. The sample processed at these conditions exhibited nano-crystalline barium hexaferrite powders with a mean crystallite size of 46 nm, mean particle size of about 200 nm and high coercivity of 334.2 kA/m.

Mn_0.4Cu_0.4Zn_0.2Fe ferrite was synthesized by soft chemical approach called co-precipitation technique. The ferrite powder was calcined, compacted and sintered at 700°C and 800°C for 3 h. The initial permeability, density, grain size, Curie temperature and dc resistivity have been studied. X-ray diffraction (XRD) method confirmed the sample to be a single-phase spinel structure without unreacted constituents. The particle size was calculated from XRD spectrum using Scherrer's formula and found to be ~55 nm. Then, nanoparticles were observed with tunneling electron microscopy (TEM). Further, scanning electron micrograph (SEM) also confirmed nano-phase and the uniformity of the particles. The initial permeability values do not exhibit much variation with temperature, except near Curie temperature, where it falls sharply. The initial permeability is found to increase with the increase in sintering temperature. This is attributed to the increase in the grain size. Calculation of activation energy indicates that the given ferrite is p-type semiconductor. Mössbauer study of these samples shows superparamagnetic behavior, which also confirms the formation of nano-particles. Possible models and mechanisms contributing to these processes have been discussed.

In this paper we have tried to develop a semi-empirical formula for estimation of starting time of reactions during mechanical alloying process according to self-propagating high temperature synthesis (SHS) mechanism. For this purpose, three SHS systems containing Ti–C, Mo–Si and Si–C were selected and their behaviors were observed. Aforementioned systems were milled in a planetary ball mill equipped with temperature sensor detector of cups. Samplings were done at different times of discontinuously milling. To change mills' energy, stainless steel and tungsten carbide balls were used. In order to detect the phases and characterizations of milled powder, XRD instrument was utilized. Results showed that all productions were synthesized after sudden increase in temperature. Maximum measured temperature and critical time had up and downtrends for production of TiC, MoSi₂ and SiC, respectively. Crystalline size of milled powder had nano-meter scale. By using experimental data along with theoretical equations, a semi-empirical formula between critical time for transformation of raw materials to productions, type of milled system and ball mill parameter can be presented with high accuracy. According to calculated formula, critical time was related to ball mill energy and Gibbs free energy of milled system with direct and inverse proportionality, respectively.

In this research, titanium alloys including smart nitinol (NiTi) were studied. The (NiTi) alloy tends to emitting (Ni) toxic ions due to its low resistance to corrosion within the body conditions over time. For (NiTi) coating process, the magnetron plasma sputtering (DC) technique was used with Aragon gas ratio of (90%) and Oxygen of (10%) in order to coat the alloy with Tantalum and its Oxide (Ta₂O${}_5)$ thin films. This is one of the methods used to improve the biocompatibility and better adhesion stability of the membrane on the (NiTi) surface, since Tantalum and its oxides are biocompatible and are not affected by the body fluids. Hardness, corrosion and biocompatibility were tested. The results showed improvement in the nominated properties using this coating technique. The hardness for the non-coated sample was (630 Kgf/mm${}^2)$, meanwhile, the coated sample recorded (762 Kgf/mm${}^2)$ using sputtering power of (25 W) with a thickness of (226 nm). Tantalum and its precipitated oxides on a pillar of thickness (90.4–226 nm) also exhibited a biocorrosion enhancement, when it was immersed in a Simulated Body Fluid (SBF). The corrosion rate for the non-coated sample was (1.204 × 10${}^{-2})$, meanwhile for the coated sample, its value was (3.453 × 10${}^{-5})$ at sputtering power of (15 W), considered as the lower corrosion rate. The scanning electron micrographs also showed an increase in the biocompatibility for the coated nitinol alloys (NiTi) in comparison with the non-coated, ones since it showed a clear formation of Hydroxyapatite (HA) on the sample surface after immersion in the SBF. This behavior was confirmed by the XRD measurements, which presented higher HA peaks on the coated samples surface in comparison with the non-coated samples.

In this paper, nano-crystalline Cu powder with a mean crystallite size of 45 nm and commercial micron-size Cu powder were either hot pressed or cold pressed and sintered conventionally to fabricate bulk samples. Hardness, density, crystallite size and microstructure of the samples after consolidation were examined. The results show that the hardness of the hot pressed nano-crystalline Cu is in the range of 0.75-1.2 GPa which is higher than that of commercial Cu. The density of the bulk nano-crystalline sample showed that the rising sintering temperature increases the density up to 97% of the theoretical value. The mean crystallite size of the hot pressed sample was 64 nm, which still was in the nano scale. The scanning electron microscopy (SEM) images revealed that the hot pressed samples contain less porosities compared to the conventionally consolidated samples.

In this study, mechanical alloying was used to produce MoSi₂ powder directly from molybdenum trioxide. Mixture of MoO₃, Si and Al powders were exposed to high mechanical activation in a planetary ball mill. The ball to powder mass ratio was constant at 33:1 and the rotation speed (cup speed) was 290 rpm during the milling operations. Phase compositions and structural evolutions during milling were investigated by X-ray diffraction analysis. The morphology of the mechanically alloyed powders was evaluated with scanning electron microscope (SEM). From XRD results, it was observed that within 3 hours of milling, MoO₃ was completely reduced and a MoSi₂-Al₂O₃ composite powder was produced. Further milling resulted in transformation of β- MoSi₂ phase to α- MoSi₂. Mean crystallite sizes in product phases in the sample milled for 30 hours calculated by Scherer method using XRD patterns were found to be less than 100 nm.

Nano-crystalline titanium diboride (TiB₂) was prepared by self-propagating high-temperature synthesis through putting a hot filament on top of the compact mixture of TiO₂, H₃BO₃ and Mg with a stoichiometric ratio. Effects of the addition of various chloride salts e.g. NaClO₄ and NH₄Cl as process control agents on phase evolution and chemical analysis and the morphology of the products were investigated by XRD and SEM techniques, respectively. Analysis of the X-ray diffraction patterns confirmed the formation of TiB₂ together with some intermediate phases such as Mg₃B₂O₆ and Mg₂TiO₄ in as synthesized powder. MgO phase was detected as a major phase in the XRD patterns. Nano-crystalline TiB₂ became the major phase in some of the leached samples by HCl. The results also showed that the powder particle characteristics were influenced by the addition of the chloride salts.

Nano/Submicron crystalline grains of about 250 nm were obtained in a metastable austenitic stainless steel AISI304L by an advanced thermomechanical process consisting of heavy conventional cold rolling and annealing. Effects of cold thickness reduction and temperature and time of the reversion treatment on microstructure and mechanical properties of the steel were investigated. The nano-structured austenitic steel exhibited not only high strength (above 1 GPa) but also good elongation (above 50%).

In this research, effect of milling time on solid state reduction of MoO₃ with carbon has been investigated. It was found that mechanical activation of a mixture of MoO₃ and carbon at ambient temperature by high energy ball milling was not able to reduce MoO₃ to metallic molybdenum. MoO₃ was converted to MoO₂ at the first stage of reduction and peaks of the latter phase in X-ray diffraction patterns were detected when the milling time exceeded from 50 hours. The main effect of increased milling time at this stage was decreasing of MoO₃ peak intensities and significant peak broadening due to decrease in size of crystallites. After prolonged milling, MoO₃ was fully reduced to nano-crystalline MoO₂ and its mean crystallite size was calculated using Williamson–Hall technique and found to be 17.5 nm.

Thermodynamic investigations also confirm the possibility of reduction of MoO₃ to MoO₂ during the milling operation at room temperature. But, further reduction to metallic molybdenum requires thermal activation at higher temperature near 1100 K.

XRD and SEM techniques were employed to evaluate the powder particles characteristics.

In this paper, the influence of toluene as the process control agent (PCA) and pre-milling on the extension of solid solubility of 7 wt.% Cr in Cu by mechanical alloying in a high energy ball mill was investigated. The structural evolution and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, respectively. The solid solution formation at different conditions was analyzed by copper lattice parameter change during the milling process. It was found that both the presence of PCA and pre-milling of Cr powder lead to faster dissolution of Cr. The mean crystallite size was also calculated and showed to be about 10 nm after 80 hours of milling.