Andrew P. Warren

Comparison of the agglomeration behavior of thin metallic films on SiO2

The stability of continuous metallic thin films on insulating oxide surfaces is of interest to applications such as semiconductor interconnections and gate engineering. In this work, we report the study of the formation of voids and agglomeration of initially continuous Cu, Au, Ru and Pt thin films deposited on amorphous thermally grown SiO2 surfaces. Polycrystalline thin films having thicknesses in the range of 10–100nm were ultrahigh vacuum sputter deposited on thermally grown SiO2 surfaces. The films were annealed at temperatures in the range of 150–800°C in argon and argon+3% hydrogen gases. Scanning electron microscopy was used to investigate the agglomeration behavior, and transmission electron microscopy was used to characterize the microstructure of the as-deposited and annealed films. The agglomeration sequence in all of the films is found to follow a two step process of void nucleation and void growth. However, void growth in Au and Pt thin films is different from Cu and Ru thin films. Residual ...

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...

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.

Classical size effect in oxide-encapsulated Cu thin films: Impact of grain boundaries versus surfaces on resistivity

A methodology is developed to independently evaluate surface and grain boundary scattering in silicon dioxide-encapsulated, polycrystalline Cu thin films. The room-temperature film resistivity for samples with film thicknesses in the range of 27 to 1 65 nm and different grain sizes (determined from approximately 400 to 1500 grains per sample) is compared to existing and empirical models of surface and grain boundary scattering. For the combined effects of surface and grain boundary scattering, the surface specularity parameter p is 0.6±0.2 and the grain boundary reflectivity coefficient R is 0.45±0.03. It is thereby shown that the resistivity contribution from grain boundary scattering is significantly greater than that of surface scattering for Cu thin films having Cu∕SiO2 surfaces and grain sizes similar to film thickness.

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.

X-Ray Photoelectron Spectroscopy Analysis of Oxygen Annealed Radio Frequency Sputter Deposited SiCN Thin Films

Thin films of amorphous silicon carbide nitride (a-SiC x N y ) were deposited in a rf magnetron sputtering system using a sintered SiC target. Films with various compositions were deposited onto silicon substrate by changing the N 2 /Ar gas ratios during sputtering. These films were annealed in dry oxygen ambient in the temperature range of 400-900°C. Subsequently these annealed films were characterized using X-ray photoelectron spectroscopy to investigate the chemical composition and oxidation kinetics at each annealing temperature. The results indicated that the oxidation of films was more gradual for the samples deposited with no nitrogen compared to the ones deposited with nitrogen.

Characterization of Pt-Ru binary alloy thin films for work function tuning

This letter describes materials and electrical characterization of Pt-Ru binary alloy metal gate electrodes for control of the electrode work function. The work function of the Pt-Ru binary alloy system can be tuned over a wide range of 4.8-5.2 eV. The results indicate that the change of film properties, i.e., resistivity, work function, and crystal structure, with composition is consistent with the equilibrium phase diagram and that the work function in the face-centered cubic and hexagonal close-packed single-phase regions is only weakly dependent on composition, whereas a strong dependence is observed in the intermediate compositional range.

Linear bolometer array using a high TCR VOx-Au film

We present a design for a low-noise bolometer linear array based on the temperature-dependent conductivity of a VOx- Au film. Typical thin film bolometers must compromise between low resistivity to limit Johnson noise and high temperature coefficient of resistivity (TCR) to maximize responsivity. Our vanadium oxide is alloyed with a small concentration of gold by co-sputtering, which gives very low resistivity and very high TCR simultaneously. The film is fabricated on an air bridge device having high thermal conductivity and small thermal time constant optimized for 30 to 60 Hz frame rates. The linear array functions as a low-power profile sensor with a modulated bias. For 1 V bias, we predict responsivity exceeding 1200 V/W. Johnson noise dominates with predicted NEP values as low as 1.0 × 10-11 W/Hz1/2. Preliminary device testing shows film resistivity below 2.5 Ω-cm with TCR exceeding -2.0%. Preliminary measurements of NEP and D* are reported.

Dual band sensitivity enhancements of a VO(x) microbolometer array using a patterned gold black absorber.

Infrared-absorbing gold black has been selectively patterned onto the active surfaces of a vanadium-oxide-based infrared bolometer array. Patterning by metal lift-off relies on protection of the fragile gold black with an evaporated oxide, which preserves much of gold blacks high absorptance. This patterned gold black also survives the dry-etch removal of the sacrificial polyimide used to fabricate the air-bridge bolometers. For our fabricated devices, infrared responsivity is improved 22% in the long-wave IR and 70% in the mid-wave IR by the gold black coating, with no significant change in detector noise, using a 300°C blackbody and 80 Hz chopping rate. The increase in the time constant caused by the additional mass of gold black is ∼15%.

Evolution of nanoscale roughness in Cu/SiO2 and Cu/Ta interfaces

Synchrotron x-ray scattering was used to study the evolution of interface roughness with annealing for a series of Cu thin films. The films were encapsulated in SiO2 or Ta/SiO2 and prepared by sputter deposition. Specular x-ray reflectivity was used to determine the root mean square roughness for both the upper and the lower Cu/SiO2 (or Cu/Ta) interfaces. The lateral roughness was studied by diffuse x-ray reflectivity. Annealing the films at 600 °C resulted in a smoothing of only the upper interface for the Cu/SiO2 samples, while the lower Cu/SiO2 interfaces and both interfaces for the Ta encapsulated films did not evolve significantly. This difference in kinetics is consistent with the lower diffusivity expected of Cu in a Cu/Ta interface (compared to a Cu/SiO2 interface) and the mechanical rigidity of the lower Cu/SiO2 interface. As a function of roughness wavelength, the upper Cu/SiO2 interfaces exhibited a roughness decay with annealing that was only 12.5% of that expected for classical capillarity dr...