The phase-equilibrium diagram for the system Nb2 0 5 -B2 0 3 was de termin ed expe rim e ntall y using the quenching techniqu e and examining the samples by optical r:nicroscopy and. x -r~r powd er diffractom etry. Th e syste m contaInS one bInary compound of approxImate composIt Ion 3Nb, Os' 8,03," which melts in congrue ntly at about 1150 0 e to H -Nb20 5 and B20 3' rich liquid. A large region of liquid immiscibility extend s, at 1 3~2 °e, from 10 mole pe rce nt Nb,Os to 65. 7 mo le pe rce nt Nb,Os.The theore ti call y calc ulated ex te nt of ImmI scIbIlIty IS In reaso nabl e agreement wIth the ex pe rImentally d etermin ed value.Key Word s : Boric oxide, immiscibility, niobium pe ntoxid e, oxid es, phase equilibri a .