Amith Darbal

Phase, grain structure, stress, and resistivity of sputter-deposited tungsten films

Sputter-deposited W films with nominal thicknesses between 5 and 180 nm were prepared by varying the base pressure prior to film deposition and by including or not including sputtered SiO2 encapsulation layers. X-ray and electron diffraction studies showed that single phase, polycrystalline α-W could be achieved in as-deposited films as thin as 5 nm. The stress state in the as-deposited films was found to be inhomogeneous. Annealing resulted in stress relaxation and reduction of resistivity for all films, except the thinnest, unencapsulated film, which agglomerated. In-plane film grain sizes measured for a subset of the annealed films with thicknesses between 5 and 180 nm surprisingly showed a near constant value (101–116 nm), independent of film thickness. Thick-film (≥120 nm) resistivity values as low as 8.6 μΩ cm at 301 K were obtained after annealing at 850 °C for 2 h. Film resistivities were found to increase with decreasing film thicknesses below 120 nm, even for films which are fully A2 α-W with no metastable, A15 β-W evident. Sputter-deposited W films with nominal thicknesses between 5 and 180 nm were prepared by varying the base pressure prior to film deposition and by including or not including sputtered SiO2 encapsulation layers. X-ray and electron diffraction studies showed that single phase, polycrystalline α-W could be achieved in as-deposited films as thin as 5 nm. The stress state in the as-deposited films was found to be inhomogeneous. Annealing resulted in stress relaxation and reduction of resistivity for all films, except the thinnest, unencapsulated film, which agglomerated. In-plane film grain sizes measured for a subset of the annealed films with thicknesses between 5 and 180 nm surprisingly showed a near constant value (101–116 nm), independent of film thickness. Thick-film (≥120 nm) resistivity values as low as 8.6 μΩ cm at 301 K were obtained after annealing at 850 °C for 2 h. Film resistivities were found to increase with decreasing film thicknesses below 120 nm, even for films which are fully A2 α-W with no...

Effect of downscaling nano-copper interconnects on the microstructure revealed by high resolution TEM-orientation-mapping.

In this work, a recently developed electron diffraction technique called diffraction scanning transmission electron microscopy (D-STEM) is coupled with precession electron microscopy to obtain quantitative local texture information in damascene copper interconnects (1.8 µm-70 nm in width) with a spatial resolution of less than 5 nm. Misorientation and trace analysis is performed to investigate the grain boundary distribution in these lines. The results reveal strong variations in texture and grain boundary distribution of the copper lines upon downscaling. Lines of width 1.8 µm exhibit a strong <111> normal texture and comprise large micron-size grains. Upon downscaling to 180 nm, a {111}<110> bi-axial texture has been observed. In contrast, narrower lines of widths 120 and 70 nm reveal sidewall growth of {111} grains and a dominant <110> normal texture. The microstructure in these lines comprises clusters of small grains separated by high angle boundaries in the vicinity of large grains. The fraction of coherent twin boundaries also reduces with decreasing line width.

Grain boundary character distribution of nanocrystalline Cu thin films using stereological analysis of transmission electron microscope orientation maps.

Stereological analysis has been coupled with transmission electron microscope (TEM) orientation mapping to investigate the grain boundary character distribution in nanocrystalline copper thin films. The use of the nanosized (<5 nm) beam in the TEM for collecting spot diffraction patterns renders an order of magnitude improvement in spatial resolution compared to the analysis of electron backscatter diffraction patterns in the scanning electron microscope. Electron beam precession is used to reduce dynamical effects and increase the reliability of orientation solutions. The misorientation distribution function shows a strong misorientation texture with a peak at 60°/[111], corresponding to the Σ3 misorientation. The grain boundary plane distribution shows {111} as the most frequently occurring plane, indicating a significant population of coherent twin boundaries. This study demonstrates the use of nanoscale orientation mapping in the TEM to quantify the five-parameter grain boundary distribution in nanocrystalline materials.

Surface and grain boundary scattering in nanometric Cu thin films: A quantitative analysis including twin boundaries

The relative contributions of various defects to the measured resistivity in nanocrystalline Cu were investigated, including a quantitative account of twin-boundary scattering. It has been difficult to quantitatively assess the impact twin boundary scattering has on the classical size effect of electrical resistivity, due to limitations in characterizing twin boundaries in nanocrystalline Cu. In this study, crystal orientation maps of nanocrystalline Cu films were obtained via precession-assisted electron diffraction in the transmission electron microscope. These orientation images were used to characterize grain boundaries and to measure the average grain size of a microstructure, with and without considering twin boundaries. The results of these studies indicate that the contribution from grain-boundary scattering is the dominant factor (as compared to surface scattering) leading to enhanced resistivity. The resistivity data can be well-described by the combined Fuchs–Sondheimer surface scattering model and Mayadas–Shatzkes grain-boundary scattering model using Matthiessens rule with a surface specularity coefficient of p = 0.48 and a grain-boundary reflection coefficient of R = 0.26.

Interfacial Strain Mapping and Chemical Analysis of Strained-Interface Heterostructures by Nanodiffraction and Electron Energy-Loss Spectroscopy

Strain engineering is a relevant optimization route to introduce and/or optimize defects for mixed ionicelectronic conducting oxides. Interfacial strain control of electrical conductivity [1] and resistive switching [2] was reported for sideways-contacted Gd0.1Ce0.9O2-δ|Er2O3 (GCO|ERO) ‘microdot’ heterostructures with alternating monolayers of insulating ERO and mixed-conducting GCO, whose lattice mismatch yielded compressive strain in the GCO layers. Here we explore these and other GCO heterostructures with alternative straining oxides that impart varying degrees of tensile strain on GCO, such as Bi4NbO8.5|GCO (BNO|GCO). We apply local strain and chemical mapping, along with high resolution imaging in the TEM and scanning TEM (STEM) to provide nanoscale insights regarding strained heterostructure design.

Correlated Electron Microscopy across Length Scales to Elucidate Structural, Electrical and Chemical Properties of Oxide Grain Boundaries

Because of their favorable ionic and/or electronic conductivity, non-stoichiometric oxides are utilized for energy storage, energy conversion, sensing, catalysis, gas separation, and information technologies, both potential and commercialized. Charge transport in these materials is influenced strongly by grain boundaries, which exhibit fluctuations in composition, chemistry and atomic structure within Ångstroms or nanometers [1-3]. Here, studies are presented that elucidate the interplay between macroscopic electrical conductivity, microscopic character, and local composition and electronic structure of grain boundaries in polycrystalline CeO2-based solid solutions. Electron energy-loss spectroscopy (EELS) in the aberration-correction scanning transmission electron microscope (AC-STEM) is used to quantify local composition and electronic structure. Electron diffraction orientation imaging microscopy is employed to assess microscopic grain boundary character, and links macroand nanoscopic techniques. These correlated experimental approaches provide unique insights into fundamental GB science, and highlights how novel aspects of nanoscale GB engineering may be manipulated to control ion transport properties in electroceramics.

On twin density and resistivity of nanometric Cu thin films

Crystal orientation mapping in the transmission electron microscope was used to quantify the twin boundary length fraction per unit area for five Ta38Si14N48/SiO2 encapsulated Cu films with thicknesses in the range of 26–111 nm. The length fraction was found to be higher for a given twin-excluded grain size for these films compared with previously investigated SiO2 and Ta/SiO2 encapsulated films. The quantification of the twin length fraction per unit area allowed the contribution of the twin boundaries to the size effect resistivity to be assessed. It is shown that the increased resistivity of the Ta38Si14N48 encapsulated Cu films compared with the SiO2 and Ta/SiO2 encapsulated films is not a result of increased surface scattering, but it is a result of the increase in the density of twin boundaries. With twin boundaries included in the determination of grain size as a mean-intercept length, the resistivity data are well described by 2-parameter Matthiessens rule summation of the Fuchs-Sondheimer and Ma...

Characterizing Texture and Grain Boundaries in Nanoscale Cu Interconnects by Precession Electron Diffraction

The constant downscaling of back-end of line Cu interconnects (CIs) has resulted in changes to their microstructure [1]. Among these changes, any variation in local texture and grain boundary types could strongly affect reliability issues like stress migration and electromigration [2, 3]. In the current work, we couple precession electron microscopy and D-STEM [4] using the ASTAR system from NanoMEGAS to obtain texture information in 180 nm and 120 nm wide damascene Cu lines with a spatial resolution of 1-2 nm. Furthermore, we perform misorientation and trace analysis using the TSL OIM software to investigate the presence of 3 boundaries, which are typically predominant in Cu, and non-CSL high angle boundaries [5].