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The LuB12 ® LuB4 ® LuB2 phase transformations on annealing in vacuum (T=(1400÷1800) K, p < 10-2 Pa) are investigated with use of the parent single crystals. SEM and X-ray researches of the corresponding lutetium boride single crystals were carried out before and after their annealing. It is shown that the LuB12 → LuB4 phase transformation takes place in surface layer and transition region spreads inwards the single crystal bulk with time. According to the assessed Lu-B phase diagram the LuB4 phase transformation into other individual phases is impossible, and at first it is shown that under corresponding conditions the LuB4 → LuB2 spontaneous phase transformation takes place both on the surface and in the LuB4 single crystal bulk.

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