The elastic moduli and flow stresses of as-deposited Pt and Pt-Ru solid solution thin films were investigated by the nanoindentation method. The influence of solid solution alloying was explored by depositing Pt-Ru solid solution thin films with various compositions onto Si substrates. The 200 nm films were prepared by DC magnetron cosputtering with a Ru composition range from 0 to 20wt%. As expected, the modulus and the flow stress both increased significantly with an increase in Ru. The experimental results compare favorably to predictions based on a simple dislocation motion model consisting of three strengthening terms: substrate constraint, grain size strengthening and solid solution strengthening.

The mechanical properties of thin metal films have been investigated for many years. How- ever, the underlying mechanisms are still not fully understood. In this paper we give an overview of our work on thermomechanical properties and microstructure evolution in pure Cu and dilute Cu-Al alloy films. Very clean films were produced by sputtering and annealing under ultra-high vacuum (UHV) conditions. We described stress-temperature curves of pure Cu films with a constrained diffusional creep model from the literature. In Cu-1at.%Al alloy films, Al surface segregation and oxidation led to a “self-passivating” effect. These films showed an increased high- temperature strength because of the suppression of constrained diffusional creep; however, under certain annealing conditions, these films deteriorated due to void growth at grain boundaries.

The microstructure of materials (grain orientation, grain boundaries, grain size distribution, local strain/stress gradients, defects, …) is very important in defining the electromigration resistance of interconnect lines in modern integrated circuits. Recently, techniques have been developed for using submicrometer focused white and monochromatic x-ray beams at synchrotrons to obtain local orientation and strain information within individual grains of thin film materials. In this work, we use the x-ray microdiffraction beam line (7.3.3) at the Advanced Light Source to map the orientation and local stress variations in passivated Al(Cu) test structures (width: 0.7, 4.1 μm) as well as in Al(Cu) blanket films. The temperature effects on microstructure and stress were studied in those same structures by in-situ orientation and stress mapping during a temperature cycle between 25°C and 345°C. Results show large local variations in the different stress components which significantly depart from their average values obtained by more conventional techniques, yet the average stresses in both cases agree well. Possible reasons for these variations will be discussed.

Cold Gas Spraying is a new coating technique, in which the formation of dense, tightly bonded coatings occurs only due to the kinetic energy of high velocity particles of the spray powder. These particles are still in the solid state as they impinge on the substrate. Adiabatic heating after impingement can cause local shear instabilities and jet formation. The local microstructure is strongly dependant on local stress state and temperature rise. A variety of different microstructures is observed by TEM. The results are compared with modelling of the spray process.

There is evidence indicating that multilayer films can be harder than monolithic ones. To investigate this, TiN/NbN multilayers with bilayer thicknesses ranging from 4 nm to 30 nm have been grown on MgO (001) single crystals using reactive magnetron sputtering. The sharpness of the interface and the composition modulation, which would be expected to strongly influence dislocation motion, have been studied by X-ray diffraction (XRD). These experiments show that the interfaces remain reasonably sharp (interface thickness ∼1 nm) and the composition modulation amplitude is maximum for multilayers with bilayer thicknesses greater than ∼10 nm. With thinner bilayers, the composition modulation decreases but the layered structure remains. Despite this, the nanoindentation hardness of the multilayers is between 20 and 25 GPa, which is similar to that of TiN and NbN alone, and therefore, no hardening due to the layering is observed. The deformation mechanisms observed under the indent in the TEM are consistent with these results.

In this work, SiGe films on low temperature Si buffer layers were grown by solid-source molecular beam epitaxy and characterized by atomic force microscope, photoluminescence and Raman spectroscopy. Effects of the growth temperature and the thickness of the low temperature Si buffer were studied. It was demonstrated that using proper growth conditions of the low temperature Si buffer, the Si buffer became tensily strained and gave rise to the compliant effect. High-quality SiGe films with low threading dislocation density have been obtained.

X-ray diffraction has been used to measure the stress, the crystallite size and the dislocation distribution in thin metal layers. By measuring two orders of a reflection, the contribution of the size distribution to the diffraction line broadening can be eliminated. A model equation is fitted to the strain Fourier coefficients of the diffraction line from which the dislocation arrangement can be obtained. For untextured nickel on steel or on silicon the dislocation densities have been obtained. It is demonstrated that for highly textured layers more information can be obtained than for untextured layers. It was found that a heated molybdenum layer on oxidized silicon showed only inclined screw dislocations.

Four-point bending experiments in combination with thermal cycling of thin films on substrates were performed in a dedicated apparatus. Strains up to ±0.8% could be imposed into Cu films of 0.2, 0.5, and 1.0 μm thickness on Si substrates by bending the substrates at various temperatures in high vacuum. After relief of the bending, the residual stress was measured by the wafer-curvature method. At temperatures below 250°C, the yield behavior is asymmetric in tension and compression. The amount of plastic strain introduced by external bending increases with film thickness, but the absolute values of the introduced plastic strains are very low throughout. At higher temperatures, there is no clear thickness dependence and no asymmetry in tension and compression. The results are discussed in connection with the formation of misfit dislocations during plastic deformation of thin films.

We have made an extensive study of Si0.82Ge0.18 film relaxation on silicon on insulator (SOI) substrates having a top Si layer 40, 70, 330nm, and 10[.proportional]m thick. SiGe films were deposited with a thickness up to 1.2[.proportional]m in an ultrahigh vacuum chemical vapor deposition system at 630°C. Following growth, films were characterized by X-ray diffraction and a dislocation revealing etch. The same level of relaxation is reached for each thickness of SiGe film independent of the substrate structure. Accompanying the film relaxation is the development of a tetragonal tensile strain in the thin Si layer of the SOI substrates. This strain reached 0.22% for the 1.2[.proportional]m film on the 40nm SOI and decreases with SOI thickness. The Si thickness of the SOI substrate also effected the threading dislocation density. For 85% relaxed films the density fell from 7×106 pits/cm2 on bulk Si to 103pits/cm2 for the 40, 70, and 330nm SOI substrates. The buried amorphous layer of the SOI substrate alters the dislocation dynamics by allowing dislocation core spreading or dislocation dissociation. The reduced strain field of these dislocations reduces dislocation interactions and the pinning that results. Without the dislocation pinning, the misfit dislocations can extend longer distances yielding a greatly reduced threading dislocation density.

Motivated by x-ray scattering experiments on heteroepitaxially grown thin films, we present model calculations of the diffuse x-ray scattering arising from misfit dislocations. The model is based on the elastic displacements from dislocations whose positions are spatially uncorrelated. These numerical results give support to a phenomenological model [Phys. Rev. B 51, 5506 (1995)] that predicts the scaling of diffuse scattering intensity with perpendicular wavevector, Qz. At low Qz the diffuse width scales inversely with the defect size, which is given by the film thickness due to the effect of the elastic image field, whereas at high Qz the diffuse width is mosaic-like, scaling with Qz. New experimental results for InxGa1−xAs/GaAs are also presented and compared to the model. The calculations are in good agreement with these experiments, as well as other measurements in the literature for high and low dislocation density.

The analysis of thickness-fringe contrast in weak-beam transmission electron microscope (TEM) images has been shown to be a reliable method for the complete determination of the character, as well as the magnitude, of a dislocation Burgers vector. By selecting multiple diffraction conditions and, for each condition, determining the number of terminating thickness fringes at the exit of a dislocation from a wedge-shaped sample, the Burgers vector can be unambiguously determined. Defect analysis of GaN pyramids grown on (111)Si by the lateral epitactic overgrowth (LEO) technique reveals a core region which contains a relatively high density of dislocations and a lateral-growth region where the defect density is decreased. The thickness-fringe contrast technique was used in the lateral growth regions of the pyramids to analyze the dislocation Burgers vectors.

Dislocation pileups with abnormally weak inter-dislocation repulsion have been observed in locally oxidized silicon structures. To verify if this could be attributed to elastic interaction of dislocations with intrinsic point defects, distributions of self-interstitials in dislocation stress fields have been studied using theoretical calculations and computer simulations. According to the obtained results, self-interstitials can form atmospheres about dislocations causing dislocation stress reduction and therefore screening of dislocations from interaction with external stresses. This may represent an additional mechanism of dislocation locking in silicon alternative to oxygen pinning.

In this study we present investigation on the anelastic behavior of sputtered 1 [.proportional]m thin Cu films. Most of the literature that reports on the mechanical properties of thin metallic films is based on substrate curvature measurements. We have developed a new version of a bulge tester that combines the capacitive measurement of the bulge deflection of a membrane with a resonance frequency measurement of the residual stress in the membrane. A Cu membrane is plastically deformed to a pre-determined strain by controlled gas-pressure bulging of the membrane. After the bulging stress is removed, the residual tensile stress, which has been decreased by the plastic deformation, is then determined by measuring the resonant frequency as a function of time. Immediately after plastic straining, the residual (tensile) stress of membranes was observed to increase. At room temperature a maximum stress was typically reached in the order of an hour. At still longer times the stress decreased again as a result of creep. The transient increase in stress following plastic straining grew larger as the amount of plastic strain produced by bulging was increased. With higher temperatures the transient became both faster and larger. A model is presented that based on the mechanism of thermally activated glide separates the microstructure in a class of “soft” and “hard” grains solving the issue of an “apparent” increase in strain energy as a function of time after deformation.

A kinetic model is presented to simulate the strain relaxation in the GexSi1−x/Si(100) systems. In the model, the nucleation, propagation and annihilation of threading dislocations, the interaction between threading dislocations and misfit dislocations, and surface roughness are taken into account. The model reproduces a wide range of experimental results. The implications of its predictions on the threading dislocation reduction during the growth processes of the heteoepitaxial thin film systems are discussed.

An approach is developed for understanding the cross-hatch morphology in lattice mismatched heteroepitaxial film growth. It is demonstrated that both strain relaxation associated with misfit dislocation formation and subsequent step elimination (e.g. by step-flow growth) are responsible for the appearance of nanoscopic surface height undulations (0.1-10 nm) on a mesoscopic (∼100 nm) lateral scale. The results of Monte Carlo simulations for dislocation- assisted strain relaxation and subsequent film growth predict the development of cross-hatch patterns with a characteristic surface undulation magnitude ∼50 Å in an approximately 70% strain relaxed In0.25Ga0.75As layers. The model is supported by atomic force microscopy (AFM) observations of cross-hatch morphology in the same composition samples grown well beyond the critical thickness for misfit dislocation generation.

Misfit dislocations at the interfaces of bilayer (Ni/Cu) and trilayer (Cu/Ni/Cu) thin films were examined by plan-view transmission electron microscopy (TEM). In the bilayers, the spacing of misfit dislocations was measured as a function of Ni layer thickness. The critical thickness, at which misfit dislocations start to appear with the loss of coherency, was found to be between 2 and 5 nm. The spacing of the misfit dislocations decreased with increasing Ni layer thickness and reached a plateau at the thickness of 30 nm. The minimum spacing is observed to be about 20 nm. A g·b analysis of the cross-grid of misfit dislocations revealed 90° Lomer dislocations of the <110>{001} type lying in the (001) interface plane at a relatively large thickness of the Ni layer, but 60° glide dislocations of the <110>{111} type at a relatively small thickness of the Ni layer. In the trilayers, misfit dislocations formed at both interfaces. The spacing of the misfit dislocation is in agreement with that of the bilayers with a similar Ni layer thickness. The misfit dislocation arrays at the two interfaces, having the same line directions, are 60° dislocations with edge components with opposite signs but are displaced with respect to each other in the two different interface planes. This suggests that interactions of the strain fields of the dislocations have a strong influence on their positions at the interface.

The strain states induced by a lattice mismatch in epitaxial systems have been studied by Transmission Electron Microscopy (TEM) using the moiré fringe technique on plane view samples. For the GaSb/(001)GaAs system, moiré patterns suggest that the GaSb layer is free of stress and homogeneously relaxed by a perfect square array of Lomer dislocations. A 10 nm thick layer of GaInAs (20% In concentration) grown on (001)GaAs does not give any moiré fringes for all low-index Bragg reflections: this result indicates that the effective misfit strain does not correspond to the theoretical one described by the elastic theory. Segregation effects are expected to play an important role in the relaxation of the misfit strain.

Recently a new microbeam bending technique utilizing triangular beams was introduced. For this geometry, the film on top of the beam deforms uniformly when the beams are deflected, unlike the standard rectangular geometry in which the bending is concentrated at the support. The yielding behavior of the film can be modeled using average stress-strain equations to predict the stress-strain relation for the film while attached to its substrate. This model has also been used to show that the gradint of stress and strain through the thickness of the film, which occurs during beam bending, does not obscure the measurement of the yield stress in our analysis.

Utilizing this technique, the yielding and strain hardening behavior of bare Cu thin films has been investigated. The Cu film was thermally cycled from room temperature to 500 °C, and from room temperature to –196°C. The film was tested after each cycle. The thermal cycles were performed to examine the effect of thermal processing on the stress-strain behavior of the film.

Mechanical stress and stress evolution in interconnections may cause reliability problems in IC circuits. It is thus of great importance to understand the origin of this stress.

In this paper, the stress evolution during the solid state reaction between blanket titanium and aluminum films has been studied by in-situ substrate curvature measurements. Whereas the formation of TiAl3 is expected to induce large tensile stress because of a global volume decrease of 6-8%, curvature measurements of titanium/aluminum dual layers during annealing at 450°C suggests the formation of a compressive compound.

The evolution of the average force per unit width of the layer during the solid state reaction is interpreted on the basis of a phenomenological model used to describe stress evolution during silicide formation.

The mechanism of plastic deformation in thin metal foils without involving dislocations was examined by investigating the variations in vacancy cluster formation during deformation for a range of deformation speeds and temperatures. The deformation morphology was not seen to change appreciably over a very wide range of strain rate, 10-4/s – 106/s, whereas the number density of vacancy clusters was observed to increase with increasing strain rate up to saturation value that is dependent on materials and temperature. The density of vacancy clusters decreased to zero with decreasing deformation speed. The strain rate at which the density of vacancy clusters begins to decrease was found to be proportional to the vacancy mobility, suggesting that the vacancies are generated as dispersed vacancies and escape to the specimen surfaces during slow deformation without forming clusters. A very long tail in the distribution of the density of vacancy clusters towards lower strain rates was reasonably attributed to the generation of small vacancy complexes due to deformation. These results give valuable information that can be used to establish new models for plastic deformation of crystalline metals without involving dislocations.