Papers by Author: U. Welzel

Abstract: The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.

Abstract: After a brief discussion of possible mechanisms of stress generation in thin film diffusion/reaction couples, two recent experimental examples are reviewed: (i) Thin film diffusion couples (Pd-Cu, individual layer thicknesses: 50nm) prepared by DC-magnetron sputtering on silicon substrates. The microstructural development, phase formation and the stress evolution during diffusion annealing have been investigated employing Auger-electron spectroscopy in combination with sputter depth profiling, transmission electron microscopy, in-situ wafer-curvature measurements and ex-situ and, in particular, in-situ X-ray diffraction measurements. (ii) Tin layers on copper substrates (layer thicknesses of some microns) prepared by electrodeposition. Upon storage at ambient temperatures, Cu diffuses into the Sn layer and forms the intermetallic phase η’- Cu6Sn5. The phase formation is accompanied by a volume expansion and as a consequence, compressive residual stresses can be generated in the Sn layers. These compressive residual stresses may drive the formation of Sn whiskers on the Sn surface. The microstructural development, phase formation and the stress evolution during diffusion annealing have been investigated employing scanning electron and focused ion beam microscopy, metallography and ex-situ and, in particular, in-situ X-ray diffraction measurements.

Abstract: Thin film diffusion couples (Pd-Cu, individual layer thicknesses: 50 nm) have been prepared by DC-magnetron sputtering on silicon substrates coated with amorphous inter-layers (Si3N4 on top of SiO2). The microstructural development, phase formation and the stress evolution during diffusion annealing have been investigated employing Auger-electron spectroscopy in combination with sputter depth profiling, ex-situ and, in particular, in-situ X-ray diffraction measurements. Upon annealing at relatively low temperatures (175°C to 250°C) for durations up to 100 hours, considerable diffusional intermixing occurs. Interdiffusion is accompanied by the sequential formation of a new phase (Cu3Pd). The detected stress changes are discussed in terms of possible mechanisms of stress generation.

Abstract: Stress gradients have been investigated employing a measurement strategy for diffraction measurements at constant penetration/information depths. Two examples have been considered: (i) sputter-deposited copper thin films on silicon wafers and (ii) γ’-Fe4N1-x layers on α-Fe substrates obtained by gaseous nitriding. In the Cu thin films rather low tensile stresses, increasing in magnitude with increasing penetration/information depth have been found. An evaluation of the measured lattice strains has been performed on the basis of the f(ψ) method, where the X-ray elastic constants (XEC’s) have been calculated as weighed averages of the corresponding Voigt and Reuss XEC’s and the weighing parameter has been taken as a fitting parameter. This evaluation reveals that the grain interaction changes with increasing penetration/information depth from near-Reuss type towards Neerfeld-Hill type. In the γ’-Fe4N1-x layers stress gradients occur due to surface relaxation near the surface and deeper in the layer due to a nitrogen concentration gradient which is built up during nitriding. First measurements in a laboratory diffractometer show the effect of surface relaxation on the stress-depth profile near the surface. As no single-crystal elastic constants are available for γ’-Fe4N1-x, the mechanical elastic constants have been employed in diffraction stress analysis. The results indicated that single-crystal elastic anisotropy occurs. From the measured data also a concentration – depth profile has been deduced.

Abstract: A rigorous strategy for (X-ray) diffraction stress measurements at fixed penetration/information depths is described. Thereby errors caused by lack of penetration-depth control in traditional (X-ray) diffraction (sin2ψ) measurements are annulled. The ranges of accessible penetration/information depths and experimental aspects are briefly discussed. The power of the method is illustrated by the analysis of an only small stress gradient in a sputter-deposited nickel layer.

Abstract: The so-called crystallite group (CGM) method, employed for diffraction stress analysis, involves that a possibly complex texture is approximated by a set of one or a few so-called ideal orientations. It has been shown that this approximation can lead to pronounced errors in the determined stress values. The range of applicability of the CGM has been investigated from a theoretical point of view. Numerical simulations of diffraction strain measurements have been performed using orientation distribution functions representing textures of different strength and sharpness. Special emphasis has been put on the fibre-textured case.