In this study, a three-step synthesis process is proposed for the production of submicron B 4 C powders. The initial step is the mechanical activation of a Mg-C-B 2 O 3 mixture, which is carried out by using a high-energy planetary ball mill. The second phase is the microwaveassisted combustion synthesis, used to fabricate the MgO-B 4 C composite powders. The final stage is an acid leaching for removing the MgO phase. The results of DSC, XRD, and SEM analyses indicated that mechanical activation was a vital process for microwave synthesis and that no starting powders were remained unreacted after microwave heating. A considerable reduction in reaction temperature was obtained from DSC analysis after mechanical activation process. TG results indicated that separated milling of Mg with B 2 O 3 powders would avoid the formation of gases during exothermic reactions. Finally, it was found that submicron boron carbide powders with an average crystallite size about 114 nm were produced with a high purity after acid leaching.
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