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X-ray powder diffraction, scanning electron microscopy, infrared spectroscopy, and elemental analysis were used to study the interaction of titanium powder with finely powdered boron of particle size 10-20 μm in Na 2 B 4 O 7 ionic melt, in the temperature range 973-1088 K, at the 5-10 h contact duration. The TiB 2 formation was shown to occur at the temperatures 1018 K or above, that is, at the borax melting temperature. According to the scanning electron microscopy, theTiB 2 powder consists of the 70-75 nm particles, and its coherent scattering region calculated from the XRD data amounts to 55 nm.