J. R. Patel

Scanning X-ray microdiffraction with submicrometer white beam for strain/stress and orientation mapping in thin films

Scanning X-ray microdiffraction (microSXRD) combines the use of high-brilliance synchrotron sources with the latest achromatic X-ray focusing optics and fast large-area two-dimensional-detector technology. Using white beams or a combination of white and monochromatic beams, this technique allows for the orientation and strain/stress mapping of polycrystalline thin films with submicrometer spatial resolution. The technique is described in detail as applied to the study of thin aluminium and copper blanket films and lines following electromigration testing and/or thermal cycling experiments. It is shown that there are significant orientation and strain/stress variations between grains and inside individual grains. A polycrystalline film when investigated at the granular (micrometer) level shows a highly mechanically inhomogeneous medium that allows insight into its mesoscopic properties. If the microSXRD data are averaged over a macroscopic range, results show good agreement with direct macroscopic texture and stress measurements.

Submicron X-ray diffraction

Abstract At the Advanced Light Source in Berkeley we have instrumented a beam line that is devoted exclusively to X-ray micro-diffraction problems. By micro-diffraction we mean those classes of problems in Physics and Materials Science that require X-ray beam sizes in the sub-micron range. The instrument is for instance, capable of probing a sub-micron size volume inside micron-sized aluminum metal grains buried under a silicon dioxide insulating layer. The resulting Laue pattern is collected on a large area CCD detector and automatically indexed to yield the grain orientation and deviatoric (distortional) strain tensor of this sub-micron volume. A four-crystal monochromator is then inserted into the beam, which allows monochromatic light to illuminate the same part of the sample. Measurement of the diffracted photon energy allows for the determination of d spacings. The combination of white and monochromatic beam measurements allow for the determination of the total strain/stress tensor (6 components) inside each sub-micron-sized illuminated volume of the sample.

Early stage of plastic deformation in thin films undergoing electromigration

Electromigration occurs when a high current density drives atomic motion from the cathode to the anode end of a conductor, such as a metal interconnect line in an integrated circuit. While electromigration eventually causes macroscopic damage, in the form of voids and hillocks, the earliest stage of the process when the stress in individual micron-sized grains is still building up is largely unexplored. Using synchrotron-based x-ray microdiffraction during an in-situ electromigration experiment, we have discovered an early prefailure mode of plastic deformation involving preferential dislocation generation and motion and the formation of a subgrain structure within individual grains of a passivated Al (Cu) interconnect. This behavior occurs long before macroscopic damage (hillocks and voids) is observed.

Quantitative analysis of dislocation arrangements induced by electromigration in a passivated Al (0.5 wt % Cu) interconnect

Electromigration during accelerated testing can induce plastic deformation in apparently undamaged Al interconnect lines as recently revealed by white beam scanning x-ray microdiffraction. In the present article, we provide a first quantitative analysis of the dislocation structure generated in individual micron-sized Al grains during an in situ electromigration experiment. Laue reflections from individual interconnect grains show pronounced streaking during the early stages of electromigration. We demonstrate that the evolution of the dislocation structure during electromigration is highly inhomogeneous and results in the formation of unpaired randomly distributed dislocations as well as geometrically necessary dislocation boundaries. Approximately half of all unpaired dislocations are grouped within the walls. The misorientation created by each boundary and density of unpaired individual dislocations is determined. The origin of the observed plastic deformation is considered in view of the constraints for dislocation arrangements under the applied electric field during electromigration.Electromigration during accelerated testing can induce plastic deformation in apparently undamaged Al interconnect lines as recently revealed by white beam scanning x-ray microdiffraction. In the present article, we provide a first quantitative analysis of the dislocation structure generated in individual micron-sized Al grains during an in situ electromigration experiment. Laue reflections from individual interconnect grains show pronounced streaking during the early stages of electromigration. We demonstrate that the evolution of the dislocation structure during electromigration is highly inhomogeneous and results in the formation of unpaired randomly distributed dislocations as well as geometrically necessary dislocation boundaries. Approximately half of all unpaired dislocations are grouped within the walls. The misorientation created by each boundary and density of unpaired individual dislocations is determined. The origin of the observed plastic deformation is considered in view of the constraints f...

Diffuse x-ray rods and scattering from point defect clusters in ion implanted silicon

We have studied the early stages of annealing in boron implanted silicon. In a grazing incidence diffuse scattering investigation of implantation-induced defects, we have observed narrow diffuse rods of intensity along 〈111〉 directions. These diffuse streaks arise from stacking faults formed during annealing in the 1000 °C range. From the width of the diffuse streak the average size of the stacking fault is 71 nm in diameter. These intensity rods are distinct from the point defect or point defect cluster scattering in the tails of the Bragg peak (Huang scattering). From the q dependence of the scattered intensity in the Huang scattering region we find clear evidence for defect clusters with an average effective size of 4 nm, remarkably independent of the annealing temperature. These observations are discussed in the context of the enhanced diffusion of implanted boron over its bulk value referred to as transient enhanced diffusion.

X-ray analysis of temperature induced defect structures in boron implanted silicon

We demonstrate the application of surface sensitive diffuse x-ray scattering under the condition of grazing incidence and exit angles to investigate growth and dissolution of near-surface defects after boron implantation in silicon(001) and annealing. Silicon wafers were implanted with a boron dose of 6×1015 ions/cm2 at 32 keV and went through different annealing treatments. From the diffuse intensity close to the (220) surface Bragg peak we reveal the nature and kinetic behavior of the implantation induced defects. Analyzing the q dependence of the diffuse scattering, we are able to distinguish between point defect clusters and extrinsic stacking faults on {111} planes. Characteristic for stacking faults are diffuse x-ray intensity streaks along 〈111〉 directions, which allow for the determination of their growth and dissolution kinetics. For the annealing conditions of our crystals, we conclude that the kinetics of growth can be described by an Ostwald ripening model in which smaller faults shrink at the...

High resolution microdiffraction studies using synchrotron radiation

The advent of third generation synchrotron light sources in combination with x-ray focusing devices such as Kirkpatrick-Baez mirrors make Laue diffraction on a submicron length scale possible. Analysis of Laue images enables us to determine the deviatoric part of the 3D strain tensor to an accuracy of 2×10−4 in strain with a spatial resolution comparable to the grain size in our thin films. In this paper the application of x-ray microdiffraction to the temperature dependence of the mechanical behavior of a sputtered blanket Cu film and of electroplated damascene Cu lines will be presented. Microdiffraction reveals very large variations in the strain of a film or line from grain to grain. When the strain is averaged over a macroscopic region the results are in good agreement with direct macroscopic stress measurements. However, the strain variations are so large that in some cases in which the average stress is tensile there are some grains actually under compression. The full implications of these observa...

X-ray diffuse scattering study of the kinetics of stacking fault growth and annihilation in boron-implanted silicon

Stacking faults in boron-implanted silicon give rise to streaks or rods of scattered x-ray intensity normal to the stacking fault plane. We have used the diffuse scattering rods to follow the growth of faults as a function of time when boron-implanted silicon is annealed in the range of 925 to 1025 °C. From the growth kinetics we obtain an activation energy for interstitial migration in silicon: EI=1.98±0.06 eV. Fault intensity and size versus time results indicate that faults do not shrink and disappear, but rather are annihilated by a dislocation reaction mechanism.

Grain orientation and strain measurements in sub-micron wide passivated individual aluminum test structures

An X-ray microdiffraction dedicated beamline, combining white and monochromatic beam capabilities, has been built at the Advanced Light Source. The purpose of this beamline is to address the myriad of problems in Materials Science and Physics that require submicron x-ray beams for structural characterization. Many such problems are found in the general area of thin films and nano-materials. For instance, the ability to characterize the orientation and strain state in individual grains of thin films allows us to measure structural changes at a very local level. These microstructural changes are influenced heavily by such parameters as deposition conditions and subsequent treatment. The accurate measurement of strain gradients at the micron and sub-micron level finds many applications ranging from the strain state under nano-indenters to gradients at crack tips. Undoubtedly many other applications will unfold in the future as we gain experience with the capabilities and limitations of this instrument. We have applied this technique to measure grain orientation and residual stress in single grains of pure Al interconnect lines and preliminary results on post-electromigration test experiments are presented. It is shown that measurements with this instrument can be used to resolve the complete stress tensor (6 components) in a submicron volume inside a single grain of Al under a passivation layer with an overall precision of about 20 MPa. The microstructure of passivated lines appears to be complex, with grains divided into identifiable subgrains and noticeable local variations of both tensile/compressive and shear stresses within single grains.

Diffuse X-ray scattering and transmission electron microscopy study of defects in antimony-implanted silicon

Ion implantation followed by laser annealing has been used to create supersaturated and electrically active concentrations of antimony in silicon. Upon subsequent thermal annealing, however, these metastable dopants deactivate towards the equilibrium solubility limit. In this work, the formation of inactive antimony structures has been studied with grazing incidence diffuse x-ray scattering, and transmission electron microscopy, and the results are correlated to previous high-resolution x-ray diffraction data. We find that at a concentration of 6.0×1020 cm−3, small, incoherent clusters of radius 3–4 A form during annealing at 900 °C. At a higher concentration of 2.2×1021 cm−3, deactivation at 600 °C occurs through the formation of small, antimony aggregates and antimony precipitates. The size of these precipitates from diffuse x-ray scattering is roughly 15 A in radius for anneal times from 15 to 180 seconds. This value is consistent with the features observed in high-resolution and mass contrast transmis...