RESUMO
The mechanical performance of electroplated Cu plays a crucial role in next-generation Cu-to-Cu direct bonding for the three-dimension integrated circuit (3D IC). This work reports direct-current electroplated (111)-preferred and nanotwin-doped nanocrystalline Cu, of which strength is at the forefront performance compared with all reported electroplated Cu materials. Tension and compression tests are performed to present the ultrahigh ultimate strength of 977 MPa and 1158 MPa, respectively. The microstructure of nanoscale Cu grains with an average grain size around 61 nm greatly contributes to the ultrahigh strength as described by the grain refinement effect. A gap between the obtained yield strength and the Hall-Petch relationship indicates the presence of extra strengthening mechanisms. X-ray diffraction and transmission electron microscopy analysis identify the highly (111) oriented texture and sporadic twins with optimum thicknesses, which can effectively impede intragranular dislocation movements, thus further advance the strength. Via filling capability and high throughput are also demonstrated in the patterned wafer plating. The combination of ultrahigh tensile/compressive strength, (111) preferred texture, superfilling capability and high throughput satisfies the critical requirement of Cu interconnects plating technology towards the industrial manufacturing in advanced 3D IC packaging application.
RESUMO
Ultrasonic slurry sampling electrothermal vaporization dynamic reaction cell inductively coupled plasma mass spectrometry (USS-ETV-DRC-ICP-MS) for the determination of Cr, Cd and Pb in several plastic samples, using NH4NO3 as the modifier, is described. The influences of the instrumental operating conditions and the slurry preparation technique on the ion signals are investigated. A reduction in the intensity of the background at signals corresponding to chromium masses (arising from matrix elements) was achieved by using NH3 as the reaction cell gas in the DRC. The method was applied to determine Cr, Cd and Pb in two polystyrene (PS) samples and a polyvinyl chloride (PVC) sample using two different calibration methods, namely standard addition and isotope dilution. The results were in good agreement with those for digested samples analyzed by ultrasonic nebulization DRC-ICP-MS. The precision between sample replicates was better than 17% with the USS-ETV-DRC-ICP-MS method. The method detection limits, estimated from standard addition curves, were about 6-9, 1-2 and 8-11 ng g(-1) for Cr, Cd and Pb, respectively, in the original plastic samples.