Composite nitrides (such as BN, TiN) are widely used in various industrial applications because of their extreme wear and corrosion resistance, thermal and electrical properties. In order to obtain composite materials with mese optimal properties, it is important to elucidate whether any chemical reactions occur at nitride/metal interfaces, e.g., those involving BN-Ti/TiN. Materials of interest include the deposition by PVD of Ti and TiN on BN substrates. Some of these systems were then subjected to varying degrees of physical and thermal alteration. Detailed X-ray photoelectron spectroscopy (XPS) has merefore been rendered of these interfaces using cross-sectional display and sputter etching. Resulting structural and morphological features have been investigated with transmission electron microscopy (TEM) and X-ray diffraction (XRD). Diffusion of the nitridation, oxynitride formation and interfacial growth are of general interest.

The vast majority of micro electro-mechanical systems fabricated today depend on polycrystalline silicon thin films for structural support. Studies involving the mechanical performance of these thin films have progressed to the point where the elastic properties and tensile strength of the films can routinely be measured using a specially designed microsample tensile testing machine. However, a fundamental understanding to predict the mechanical behavior of the polycrystalline silicon films requires that these experimental measurements be complemented with detailed observations of the underlying thin film microstructure. This paper describes some of the plan view and cross-section transmission electron microscope observations that have been performed on different deposition runs of double layer polycrystalline films obtained from the Microelectronics Center of North Carolina. The emphasis has been placed on determining the flatness and dimensions of the polycrystalline films, grain morphology and distribution, texture, and dislocation substructure and microtwinning in the undeformed films.

A system for acquisition and interpretation of Kikuchi patterns with computer-controlled electron microscopes is presented. It enables interactive as well as fully automated determination of individual grain orientations. Special features for automated crystal orientation mapping (ACOM) with the scanning electron microscope (SEM) are digital beam scan, autocalibration and dynamic focus controlled by the computer. With the present setup about three orientations per second can be measured unattendedly. In the transmission electron microscope (TEM) the on-line determination of Burgers vectors and identification of deformation systems are based on crystal orientation measurement. The characterization of dislocations is facilitated by the simulation of diffraction patterns on the computer as a function of specimen tilt.

Crystal orientation maps are obtained by assigning to the raster points in the image a color specific for the grain orientation, the misorientation or character of the grain boundary. The dala set of grain orientations is used to calculate the Schmid factors grain by grain, the orientation distribution function (ODF) and the correlated as well as the uncorrelated misorientation distribution functions (MODF) which characterize crystallographic texture in a statistical sense.

Applications of individual grain orientation measurement are:

. Thermomechanical hillocks in aluminum metallization layers on silicon substrates

. Stress-induced grain growth in aluminum metallization layers on silicon substrates

. Electromigration voids and hillocks in aluminum interconnects

A working hypothesis for electromigration failure, based on experimental findings, is discussed

The stress state of evaporated Ag films prepared on Ti underlayers before and after encapsulation process has been studied by x-ray diffraction using a “sin2ψ” technique. A low tensile stress of approximately 61 MPa was measured in the as-deposited Ag films. The stress was caused by nonequilibrium growth during film deposition and resulted in a lattice tension state in the film plane and a lattice compression state along the film normal. Thermal mismatch stress was produced by the encapsulation process at 600 °C, but most of this stress relaxed during the cooling stage, and a residual tensile stress of ∼ 320 MPa in the film plane was determined.

Multilayers and superlattices are of great industrial interest because of their specific properties (magnetic, electronic, tribological…). Multilayers stacking are often in a very high state of intrinsic stress (some GPa) and for reliable integrated devices to be made it is capital to control and understand these intrinsic as well as extrinsic stresses. The objective of the present work is therefore the understanding of the origin of stresses and strains in multilayered metallic materials. Of course, a comparison of the different techniques which can be used for stress determination is a necessary first step of this study. In this aim, we have studied Ag/Ni multilayers, Ag and Ni thin films and Ag/Ni bilayers obtained by sputtering. The stresses have been determined via curvature measurement using both a laser scanning method and X-ray diffraction rocking curves technique, and via X-ray diffraction measurement of several d-spacings which act as in-situ strain gauges (also called the sin2ψ method and related methods). The obtained results from these different techniques are discussed in terms of accuracy, reproducibility and advantages / drawbacks. The obtained stresses from these methods cannot be directly compared and a specific discussion is developed around the relation between the measured strains and stresses and the microstructure of the materials.

The relation between electromigration and microstracture for three types of Al lines with different microstructures has been studied. The lines were made by recrystallization of Al in a SiO2 groove pattern. They were either truly bamboo with grains of on average 3 μm long or distorted (i.e. with dislocations) single-crystals. In addition, conventional, polycrystalline Al lines with grains of on average 230 nm were made. The lines were lifetime-tested (200 °C,j=2, 5 and 8 MA/cm2) and subjected to 1/f noise measurements (from 200 to 500 K).

The bamboo and single-crystalline Al lines showed the same, although weak, 1/f noise. This observation demonstrates that other mechanisms than thermal motion of atoms at grain boundaries can cause noise. It is suggested that dislocations are the sources for noise in our samples. The measured activation energy (0.8 eV) is in agreement with the activation energy for pipe diffusion along dislocation lines.

The lifetime-tests showed significantly higher times to failure for the single-crystalline and bamboo lines as compared to polycrystalline lines. Preliminary results indicate slightly higher lifetimes for the bamboo than for the single-crystalline lines. It is concluded that interface diffusion is the main mechanism for electromigration in truly bamboo or single-crystalline lines. Our measurements demonstrated that dislocations are important in the formation of 1/f noise and interfaces in the formation of electromigration damage.

Novel metal deposition stack and damascene processing methods have been used to fabricate electrically isolated parallel arrays of 1.0 νm deep aluminum-alloy interconnect trenches varying in width from 0.5 μm to 16 μm. The grain size and crystallographic texture of the Al in these trenches has been characterized using transmission electron microscopy (TEM) and local electron backscattered diffraction (EBSD), respectively. Narrow lines (0.5 and 1.0 μm wide) have a bamboo microstructure, intermediate widths (2.0 μm wide) are nearly bamboo, and wide lines (4.0 μm and wider) are polycrystalline. The <111> texture of the lines degrades with decreasing linewidth. A secondary <100> component is demonstrated and its origin proposed. The electromigration reliability of the narrow damascene Al lines was measured, and the observed enhancement of damascene Al interconnects compared to conventionally-fabricated Al interconnects is correlated with the microstructure.

The electromigration lifetime of aluminum interconnect lines shows a strong dependence on the quality of the texture in the metal. This observation has been explained in terms of a decreased diffusivity along the grain boundaries, generally the dominant path for diffusion and void growth. As the texture in the metal is strengthened, atomic order along the grain boundaries is increased, and diffusion is suppressed.

In this paper, we examine passivated A1–0.5wt%Cu interconnect lines having either TaAl underlayers or conventional Ti/TiN underlayers. Rocking curve measurements confirm that Al deposited on TaAl has a very strong (111) texture (FWHM ∼ 0.6°) compared to Al on Ti/TiN (FWHM ∼ 6°). Interconnect lines of both types were electrically stressed at 225°C and 250°C for 20 hours at a current density of 3 MA/cm2. The lines were then stripped of passivation, and the void numbers, sizes, and morphologies were determined.

Analysis of the void data gave a surprising result: the void volume in the highly-textured Al was greater than in the conventional Al. However, voids in the conventional Al were observed to follow grain boundaries across the width and sever the line, while such destructive void growth was not observed in the highly-textured Al. Instead, voids grew either with a faceted shape or along the line edge, never extending across the line width. Modeling electromigration in the surrounding microstructures shows that void locations in the highly-textured lines are often independent of the surrounding grain boundaries. In this case, the line sidewalls appear to be significant mass transport paths. Since these paths do not cross the line width, voids growth across the line is difficult. This resistance to fatal damage makes highly textured aluminum a promising interconnect material.

PVD-TixSiyNz films formed by reactive RF-magnetron co-sputtering of Ti and Si in Ar/N2 are evaluated as a diffusion barrier between Cu and Si. A complete range of compositions are obtained by Ti targets inlaid with Si. Film composition is controlled by the target ratio of titanium to silicon and N2 partial pressure. Electrical results versus thermal history for films of∼6–18% Si as well as the composition and microstructure as determined by Rutherford back scattering (RBS), TEM and electron diffraction are reported. These films are an amorphous matrix with imbedded nanocrystals of titanium nitride as-deposited and undergo phase separation to yield titanium nitride and silicon nitride after a 1000°C anneal. As-deposited compositions which lie above the TiN-Si3N4 phase line yield crystals of TiN. Compositions below the TiN-Si3N4 phase line yield crystals of Ti2N. Bulk resistivity as-deposited (<400μΩ2-cm) is acceptable for use as a contact liner/berrier material and improves with annealing. Si pn-diodes metallized with 20nm Ti40Si15N45 and Cu show no significant increase in reverse leakage current at anneal temperatures below 700°C.

Amorphous Ta-Si-N thin film was deposited by dc sputterring of Ta5Si3 target in (Ar+N2) atmosphere. The crystal structure and the thermal stability of Ta-Si-N thin films were investigated by XRD, RBS, AES, Nomarski microscope, and TEM. When the concentration of nitrogen in Ta-Si-N thin film was higher than 40 at.%, the Ta-Si-N thin film remained the amorphous state after the annealing at 1100°C for 60 min. In this case, the Cu diffusion was prevented by the amorphous Ta-Si-N thin film even if the annealing temperature increased up to 900°C for 30 min. Whereas, the Ta-Si-N thin film with nitrogen concentration less than 40 at. % was transformed from the amorphous to the polycrystalline TaSi2 phases after the annealing at 900°C for 60 min and failed to prevent the Cu diffusion after the annealing at 700°C for 30 min.

We present and discuss experiments designed to demonstrate the effects of ramping substrate temperature during the deposition of TIBA sourced aluminum on Si(100) and TiNx coated silicon (TiN) wafers. We also present results from experiments in which the precursor flow was pulsed (started and stopped) for a short time at a higher temperature followed by temperature ramp down and deposition at a lower (constant) temperature on TiN wafers. Aluminum growth rates and crystal orientation data are presented for different deposition conditions on Si(100) wafers. Aluminum nucleation densities, crystal orientation, average grain size, surface roughness, growth rate and resistivity data are presented for different deposition conditions on TiN wafers. During substrate temperature ramp down from 673 K on TiN wafers, when the precursor flow was pulsed for a short time at higher temperatures, and then resumed at a lower (constant) temperature 573 K, there was a significant increase in both deposition rates and fraction of (111) orientation. The resistivities of these films were close to that of bulk aluminum. Films deposited during substrate temperature ramp down on TiN substrates resulted in higher fractions of (111) oriention and higher resistivities as compared to the films deposited at constant substrate temperature and during the ramp up of substrate temperature. The films deposited on Si(100) wafers during substrate temperature ramp down from 673 K to 573 K had strong Al(200) orientation.

In this paper, we report on the experiment results of wet oxidation of Si1-xGex on SiO2. AES and XPS measurements were performed to study the effect of the oxidation on the Si1-xGex layer. A possible mechanism was proposed.

Real-time ellipsometry has shown to be a powerful tool to analyze thin films during processing. It is non-disturbing and its sensitivity lies in the submonolayer range. In fact, a slight variation in the film microstructure might result in a significant change of the polarization state of the reflected beam from the sample surface. SiNx layers have been grown on glass, quartz, KC1 and Si substrates by laser ablating a Si3N4 sintered target in vacuum and N2 environment. The film growth was monitored by real time ellipsometry at a fixed wavelength, and a fixed incidence angle. Once the deposition process is completed, the refractive index was obtained by perfoming in situ spectroellipsometric measurements in the 1.5 to 5 eV photon-energy range. The best curve fitting of the experimental data is used to find the film composition: a mixture of Si3N4, polycrystalline Si, and amorphous Si. The films composition and micro structure inferred from ellipsometric data are compared to those obtained by in-situ surface techniques and TEM, respectively.

Ferroelectric thin films of tungsten bronze lead barium niobáte (PBN) were fabricated by radio frequency magnetron sputtering. Oriented growths of the thin films were observed along (001) in tetragonal phase and along (002) in orthorhombic phase. Excess amount of PbO (6 wt %) in the PBN targets were used to compensate Pb evaporation during sputtering deposition. Ferroelectric properties were investigated as a function of annealing temperatures. The thin film with high quality was annealed at 650 °C, while its remnant polarization (Pr) and coercive field (Ec) were equal to 47.9 μC/cm2 and 5.2 kV/cm, respectively.

A method for tensile testing thin gold films is presented. Free-standing tensile specimens were prepared by evaporating 0.8 μm of gold onto a patterned oxidized silicon wafer. Using common microelectronic fabrication techniques, free-standing thin film specimens were produced that span rectangular windows in the wafer. The wafer was diced into individual tensile specimens composed of a thin film surrounded by a silicon frame. The final step before testing was to cleave the silicon frame so that the load was completely carried by the metal film. The ultimate tensile strength of the films was found to be approximately 150% greater than that of annealed bulk gold. In contrast, the measured elastic modulus for the thin film specimens was approximately the same as that documented for bulk gold.

Microstructural control is a critical issue in the use of diamond films in a variety of engineering applications. Using a novel, electrostatic-based particle seeding process, we have investigated the deposition of diamond films with varying areal nucleation densities. Depositions were performed at 1.000 Torr in a modified electron cyclotron resonance plasma system. Methyl alcohol was the primary diamond precursor species. SEM and Raman spectroscopy were used to evaluate microstructure and composition characteristics. Comparisons in deposition characteristics were made based on relative nucleation density.

Reactive pulsed laser deposition has been used to deposit IrO2 thin films on both SiO2 and fused quartz substrates, by ablating a metal iridium target in oxygen atmosphere. At a KrF laser intensity of about 1.7 × 109 W/cm2, IrO2 films were deposited at substrate deposition temperatures ranging from room-temperature to 700 °C under an optimum oxygen ambient pressure of 200 mTorr. The structure, morphology, electrical resistivity and optical transmission of the deposited films were characterized as a function of their deposition temperature (Td). High quality IrO2 films are obtained in the 400–600 °C deposition temperature range. They are polycrystalline with preferred orientations, depending on the substrate, and show a dense granular morphology. At a Td as low as 400 °C, highly conductive IrO2 films with room-temperature resistivities as low as (42±6) μΩ cm are obtained. Over the 300–600 °C Td range, the IrO2 films were found to exhibit a maximum optical transmission at 450 °C (∼ 45 % at 500 nm for 80 nm-thick films).

Single crystal cubic boron nitride(cBN) was heteroepitaxially grown on a seed crystal of diamond under static high pressure and high temperature of 5.5GPa and 1600–1700°C, respectively, for 10–100 hour. A temperature gradient method was employed for the crystal growth by using lithium boron nitride as a solvent. Initial growth feature of cBN crystal was found on the diamond seed surface after the growing time of 10 minutes. The nucleation sites of the crystals seem to be near the etch pits on the diamond surface which were introduced by the surface dissolution by the solvent for cBN growth. Two types of growth features, island and step growth were typically shown on the surface. It can be seen that grown crystal appearing as a (111) nitrogen face was exhibited with the step growth feature, while the (11n) face exhibited the island growth feature. Considering the growth process under constant P-T growing condition, growth rate of cBN crystal was significantly small as compared to that of diamond.

PLZT(X/70/100) thin films on MgO(100), Pt/Ti/MgO(100), and Pt/Ti/Si(100) have been prepared by RF-magnetron sputtering process from sintered target with compositions of PLZT(X/70/100), where X=5, 10, and 15, respectively. The effects of substrate temperature, substrate and gas pressure on deposited thin films were studied. Crystalline and surface characterization was analyzed using XRD, SEM, AES, and AFM. X-ray rocking curves were measured to examine the film orientation. It was observed that the gas pressure was the dominant influence on having (001) preferred orientation. As a result, the degree of c-axis orientation increased as gas pressure decreased.

High resolution electron microscopy has been used to characterize the structure of ultra thin films of titanium deposited on KBr substrate by Ultra High Vacuum (UHV) electron-gun evaporation. The size of the grains has an order of magnitude of 10 nm whatever the substrate temperature. The observations have been carried out along <1123> zone axis. Some of the grains contain planar defects which were identified as the twin {1011}. The atomic structure of this twin is characterized by a mirror plane similar to that observed in polycrystalline titanium. Additionaly, this structure can be modified by a b2/2 twinning dislocation.