We examined relaxation and crystallization behavior of the ternary Zr 50 Cu 40 Al 10 metallic glass by using positron annihilation and transmission electron microscopy (TEM). Observed changes in positron annihilation lifetime of the alloy annealed isothermally at 673 K, which is below the glass transition temperature, correlate well with observed density changes; while coincidence Doppler broadening (CDB) spectra exhibit no significant change. These observations demonstrate that free volume decreases without a rearrangement of atoms during structural relaxation. On the other hand, CDB spectrum has exhibited considerable changes when the same alloy was annealed at 773 K. TEM observations suggested that crystallization occurs via growth of spherulites of several hundred nm in diameter, which themselves are composed of radially grown grains. Chemical analysis revealed that Cu atoms are partitioned out during the growth of the spherulites. Diffraction study indicated that the unit cell of the crystalline phase belong to an orthorhombic system with a ¼ 0:892, b ¼ 0:550, and c ¼ 1:060 nm; while remaining interspherulite regions are found to crystallize into an fcc phase with a ¼ 1:28 nm, which is probably isostructural to the 3 phase.
In this study, we investigated mechanical deformation-induced Sn whisker growth, which is frequently encountered in advanced flexible substrate packaging. Concentrated compressive stresses are introduced around the leads and solder surface finish joints connected by compression fixing. Six types of pure Sn thin films were electroplated on Ni-protected Cu substrates. These were 2- and 6-μm-thick Sn films electroplated with three different current densities: 2, 10, and 20 A/dm2. These films were compressed at room temperature and ambient humidity. The surface and cross-sectional grain morphologies of the films were examined by scanning electron microscopy and focused ion beam spectroscopy, respectively. The grain orientations of the electroplated Sn films were analyzed by x-ray diffraction and electron backscatter diffraction. After compression, nodule hillocks and whiskers were found around the indents. Beneath the indents, the original columnar Sn grains were deformed, and recovery and recrystallization processes occurred. Rapid whisker formation was observed. The whiskers induced by mechanical deformation are closely related to the grain microstructures, and the initial compression stresses are critical to the types and distribution of whiskers as well.
The development of the microstructure of mechanical-deformation-induced Sn whiskers on electroplated films has been examined using a focused ion beam system (FIB). The 6-lm-thick matte Sn films were compressed by using a ZrO 2 ball indenter under ambient conditions. After compression, tin whiskers and small nodules were found adjacent to, and several grains further away from, the indents. The cross-sectional microstructures of the indents and whiskers indicate that the lateral boundaries of the newly created grains caused by recrystallization are the main routes for stress relaxation.
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