Elsevier

Ceramics International

Volume 38, Issue 2, March 2012, Pages 1353-1357
Ceramics International

Synthesis of MoSi2–TiC nanocomposite powder via mechanical alloying and subsequent annealing

https://doi.org/10.1016/j.ceramint.2011.09.012Get rights and content

Abstract

MoSi2–30 wt.% TiC nanocomposite powder was successfully synthesized by ball milling and following heat treatment. Effect of milling time and annealing temperature were investigated. The products synthesis and reactions progress were characterized by XRD. Morphology and microstructure of milled powders were monitored by SEM and TEM, respectively. Results showed that the synthesis of this composite begins after 10 h of milling and progresses gradually up to 30 h of milling. MoSi2–TiC composite was completely synthesized after annealing of 30 h milled powder at 900 °C. On the basis of Reitveld refinement method, the mean grain size and microstrain of 13.2 nm and 0.44% were obtained, respectively for 30 h milled powder that is in consistent with TEM image. In the spite of grain growth and strain release, this nanocomposite powder maintained its nanostructure after annealing.

Introduction

MoSi2 is a very promising intermetallic compound as a high-temperature structural material because of its much higher melting point of 2030 °C. At present, it is mainly used as a heating element of furnaces operating in air at temperatures as high as 1750 °C, but many studies indicated that materials based on MoSi2 had a wide variety of high-temperature structural applications such as high-temperature heat exchanger, turbine aircraft engine hot-section components like blades, vanes, combustors and nozzles, automotive turbocharger rotors and valves [1], [2], [3], [4]. Its oxidation resistance at high temperatures is excellent, clearly the best of the silicides and nearly as good as silicon carbide SiC due to the formation of protective silicon dioxide SiO2 layers.

However, MoSi2 has the intrinsic disadvantages such as low fracture toughness at room temperature and poor tensile creep resistance at high temperature. Therefore, it is imperative to increase the room temperature fracture toughness and high-temperature tensile creep resistance of monolithic MoSi2 by means of proper strengthening and toughening [5]. Fortunately, it is feasible to improve the high-temperature mechanical properties of monolithic MoSi2 by the introduction of a suitable second phase such as SiC, Al2O3, Si3N4, CrSi2, and TiC [6], [7], [8], [9], [10], [11], [12], [13], [14].

Another possible mechanism to improve mechanical properties is to prepare these materials in nanostructure. MoSi2–TiC nanocomposite can be produced easily by direct mixing of its components [15], [16], [17], [18], [19]. But the resulting heterogeneous microstructure and high cost of the starting materials are two important setbacks of this method. Alternatively, MoSi2–TiC nanocomposite powder can be synthesized through high-energy reactive milling of mixtures of Mo, Si, Ti and C powders. Mechanical alloying (MA) has been used for preparing thermally stable metallic glasses and amorphous alloys, nanocrystalline and nanocomposite materials, and refractory hard materials, carbides, and hydrides [20].

The aim of this work is in situ synthesis of MoSi2–TiC nanocomposite powder by mechanical milling of its elemental powders. Formation of this composite will be studied by thermodynamic discussions and its microstructure will be investigated by Reitveld refinement method.

Section snippets

Experimental procedures

Mechanical alloying (MA) was performed in a planetary ball mill at approximately room temperature and vial rotation speeds (cup speed) 750 rpm. The four cup planetary ball mill of Retch Company was used for MA experiments. Pure Merck Mo (99.7 wt.%), Si (99.8 wt.%), Ti (99.0 wt.%) and graphite (99.3 wt.%) were mixed to give the desired MoSi2–30 wt.% TiC composition. The used starting powders have a narrow size distribution with the mean particles sizes of 50, 25, 30 and 10 μm, respectively. The ball to

Milling and annealing

Synthesis possibility of MoSi2–TiC composite powder was studied by mechanical alloying of Mo, Si, Ti and graphite elemental powders on the basis of following reactions [23]:Mo+2SiMoSi2ΔGT°=131,800+65.1T(J/mol)Ti+CTiCΔGT°=183,050+10.1T(J/mol)The starting powders were mixed to give the desired composition of MoSi2–30 wt.% TiC. Fig. 1A shows the XRD pattern of this mixture before milling. Intensity decreasing, peak broadening and disappearing of some peaks are the effects of 10 h milling. It

Conclusion

Effect of milling time and annealing temperature were investigated on the synthesis of MoSi2–TiC nanocomposite from its elemental powders. Results showed that this composite was incompletely synthesized after 30 h of milling. On the other hands, this composite was successfully synthesized after annealing of 30 h milled powder at 900 °C. SEM images showed that a very fine and submicron particles with spherical morphology were obtained after 30 h of milling. On the basis of Reitveld refinement

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