Journal of Advanced Materials in Engineering (Esteghlal)

---

In the present study phase transformation of silicon and silica during milling in different atmospheres was investigated. The silicon powder was subjected to high energy ball milling in ammonia (25%) atmosphere. The milled powder was subsequently annealed at 1200 ◦C for 1 hour. In another test a mixture of AlN and amorphous silica (micro silica) was subjected to high energy ball milling. The milled powder mixture was subsequently annealed at 1200 ◦C for 2 hours. Phase analysis of the as milled and annealed powders was performed by X-ray diffractometery (XRD). Powder morphology was also examined using a scanning electron microscope (SEM). Results showed that ball milling of silicon in ammonia formed an amorphous phase which transformed to quartz on further milling. After annealing quartz, cristobalite and another oxide phase called O phases were developed on XRD patterns. Ball milling of AlN and amorphous silica led to the transformation of amorphous silica to stishovite phase. This process was completed after annealing..

---

A powder mixtures of 18.72% wt, 17.67% wt Al2O3 and 63.6% wt zircon were prepared and milled in a planetary ball milled for one up to 10 hours in presence of air. After removal Iron impurity from as-milled samples, they were isothermally heated in temperature range of 1300-1450 0C for one hour in an air atmosphere. After cooling the samples, they were studied using XRD analyses. The XRD and PSA analyses were showed that the size of particles in the mixtures decreased with increasing of milling time and the mixtures became amorphous nature. The isothermal runs observed that pre-milling on the mixtures has great effect, wherever the zircon decomposition temperature and mullite formation temperature decreased to about 1300 0C in a one-hour-milled sample. The amount of tetragonal zirconia increased with increasing in milling time at 1300 0C, however the amount of tetragonal zirconia decreased with increasing of temperature up to 1450 0C. The amount of tetragonal zirconia at 1300 0C in the three hours milled samples was the highest value among all samples.

---

In the present study, pure Aluminum powder with 5%wt Titanium Dioxide was mechanically milled at different times. Using phase analysis through X-ray diffraction (XRD), it was found that increasing of the milling times over 10 hours causes the reduction of Titanium by Aluminum and formation of Al2O3 in the structure. Also, it was shown that if the process persists, Aluminum reacts with Titanium and causes the formation of Al3Ti in the composition. The reactions were studied through the thermodynamic relations. Furthermore, after distribution of reinforcement particles in the matrix, using X-ray diffraction peak broadening, according to Williamson-Hall equation, the mean crystallite size and lattice strain were determined, and by scanning electron microscopy (SEM), the structure and morphology of the powder particles were studied.

---

Silicon nitride has attracted a considerable attention because of its excellent properties such as high-temperature strength, good oxidation resistance, high corrosion resistance, good thermal shock resistance, high creep resistance and good thermal and chemical stability. There are several different fabrication methods for synthesizing Si3N4 particles. Such methods are mostly costly and kinetically slow and require lengthy heat treatment. In this study, Si3N4 compounds were synthesized by means of mechanical milling. In the mechanical milling route,Si powder (≤99.0%) was milled under nitrogen gas for 25 h and heated at various temperatures 1100-1200-1300 and 1400 C for 1 h at the nitrogen atmosphere at a rate of 200 ml/min. Silicon powder was also annealed under a similar condition in order to evaluate the impact of milling process on the low temperature synthesizing of Si3N4. Phase identification and microstructural characteristics of products were evaluated by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. The Fourier transform infrared spectroscopy and thermal analysis were used for characterization of the formed bands and thermal treatment of the sample, respectively. The obtained results exhibited that Si3N4 powder was fully formed with two kinds of morphologies including globular particles and wire with a width of 100–300 nm and length of several microns at sintering temperature of 1300 C. This was confirmed by the Si–N absorption bonds in the FTIR trace. Based on XRD results, 25 h milling reduced temperature of reaction remarkably in comparison with direct nitridation of Si powders for 1 h. With an increase in the reaction temperature, the Si3N4 samples had a phase transformation 𝛂→𝛃, and variation of the morphology followed the vapor–liquid -solid mechanism.