Authors: Maria José Marques, J.C.P. Pina, A. Morão Dias
Abstract: The conventional Bragg diffraction geometry, normally used to characterize the residual
surface stress state, it is not suitable to evaluate surface treated materials and thin films. The X-ray
path lengths through a surface layer or thin film are too short to produce adequate diffraction
intensities in relation to the bulk or the substrate. Another limitation of the conventional technique
appears when a residual stress gradient is present in the irradiated surface. The technique only
enables the evaluation of the mean value of this gradient. In these cases, a recently proposed
Pseudo-Grazing Incident X-ray Diffraction method would be better applicable.
In this study, the Pseudo-Grazing Incidence X-ray Diffraction is applied to characterize the residual
stress depth profiles of several AISI 4140 samples, which were prepared, by mechanical polishing
and grinding, in order to present different surface roughness parameters, Ra. The experimental
results lead to the conclusion that the surface roughness limits the application of the
Pseudo-Grazing Incidence methodology to a minimum X-ray incident angle. This angle is the one
that enables a mean X-ray penetration depth with the same order of magnitude of the sample surface
roughness parameter, Ra.
1618
Authors: J.C.P. Pina, Maria José Marques, J.M.M. dos Santos, A. Morão Dias
Abstract: The thin and textured coatings present a double difficulty for characterization by
conventional X-ray diffraction. Their shallow depth reduces the diffracted intensity and allows the
interference of the underlying material. Frequently they present a crystallographic texture which
limits the number of orientations that provide good intensity and induces anisotropy effects on their
mechanical behavior. Reliable results can be determined using diffraction geometry of lowincidence
angle. This paper describes the application of the technique to several films, characterized
by thicknesses of the order of 1 μm and crystallographic textures. Examples are proposed of
chromium films applied by PVD on molybdenum substrates, decorative electroplated coatings, and
aluminum coatings used for interconnections in microelectronic circuits. The Cr films are 1.5 μm
thick and exhibit a strong <100> fiber texture. The decorative coatings were studied both on the
nickel undercoat and in the Cr top layer. Results are presented for chromium where tensile stresses
and a <110> fiber texture were observed. The Al films are 1.0 μm thick. Some samples were heattreated
at different annealing temperatures. Tensile stresses were always observed, which increase in
the annealed samples.
1613
Authors: J.M.M. dos Santos, J.C.P. Pina, António Castanhola Batista, Alton B. Horsfall, Kai Wang, Nicolas G. Wright, S.M. Soare, S.J. Bull, Anthony G. O'Neill, J.G. Terry, Anthony J. Walton, A.M. Gundlach, J.T.M. Stevenson
Abstract: The evaluation of stress in sub-micron tracks is critical for the microelectronics industry and there is a need for new methods of measurement. This paper advocates the use of a rotating beam sensor structure which can be fabricated on the wafer along side electronic devices and used to monitor stress generation and relaxation as a function of processing. The rotation can be observed with a reflected light microscope and correlated to the actual stress level. Several samples, assputtered and sintered, were prepared with the aim of having different residual stress states. X-ray diffraction with a low incident angle geometry, was used to evaluate the residual stresses on the aluminum layer. Computer simulations using ANSYS were also performed in order to correlate the sensor rotation with the experimental stress values. It was observed that the extrinsic stress from the
mismatch in expansion coefficients between the aluminum layer and the silicon substrate dominates over the compressive stress from the sputter growth. Sintering the layers at temperatures above 150°C reduces this compressive stress due to the action of creep. The calibration of the rotation of the device with the direct measurements of the X-ray diffraction shows that the sensor has a resolution better than 2.8 MPa.
649
Authors: P. Matos, Pedro Miguel Guimarães Pires Moreira, J.C.P. Pina, A. Morão Dias, Paulo Manuel Salgado Tavares de Castro
Abstract: Cold working introduces a compressive stress field around rivet holes, reducing the
tendency for fatigue cracks to initiate and grow under cyclic mechanical loading. As it is well known, for the accurate assessment of fatigue lifetimes a detailed knowledge of the residual stress profile is required. Powerful experimental and numerical tools are nowadays available for that purpose. In the present work both types of tools, X-ray diffraction and 3D Finite Element Analysis (FEA), were used
in order to evaluate the residual stress profile. A comparison of experimental and numerical data is presented and discussed.
41
Authors: J.C.P. Pina, A. Morão Dias, Jean Lu Lebrun
683
Authors: C. Veiga, Altino Loureiro, J.C.P. Pina, António Castanhola Batista
387