A bulk glass Zr 52.5 Ni 14.6 Al 10 Cu 17.9 Ti 5 alloy with 6 mm diameter is prepared by pre-melting sponge zirconium together with other pure metal elements and followed by injecting cast. In the samples, the content of oxygen is chemically analyzed in the level of 706 ppm (atomic concentration), which significantly affects the crystallization and the microstructure. When the bulk glass samples are annealed at the temperature far below the crystallization temperature( T x ), the predominant phases of Zr 2 Ni 0.67 O 0.33 and Zr 2 Ni compounds crystallize and uniformly distribute on glass matrix. These predominant phases will grow and join together to form net-shape phase when the annealed temperature is in the range of T x to above T x . The glass matrix phase separated by the net-shape phase into the size of about 25 μm at 703 K to 15 μm at 823 K almost fully transforms into Zr 2 Ni and a small amount of Zr 2 Cu and Zr 4 Al 3 . At annealing temperatures far above T x , Zr 2 Cu and Zr 4 Al 3 compounds crystallize by phase separation to form nanostructure with nano-scale phases of Zr 2 Cu and Zr 4 Al 3 compounds distributed on the matrix of Zr 2 Ni. The micro-compressive tests by Nanoindenter II reveal that the bulk glass phase has a lower elastic modulus and lower microhardness. Increasing the annealing temperature, the modulus and microhardness for the crystallized microstructure increase. With the phase separation taking place, the modulus and microhardness for the nanostructure are improved slightly. But the different deformational mechanism between micro-scale and bulk specimens is unknown.
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