Three families of NixZry (x = 28, 36, 38, x + y = 100%) metallic glasses were prepared and examined using X-ray, temperature dependent transport and magnetic field. X-ray characterization shows characteristic diffuse spectrum, except for narrow regions of control samples, where partial crystallization was induced in finite small volumes. Magnetic properties confirm spin-fluctuating paramagnetic-like behavior, which we asses from preliminary Hall coefficient measurements, which is quantitatively different in three sample families. Temperature dependent AC and DC transport measurements were conducted in a broad temperature range from 70 K to 700 K, finding both quantitative and semi-qualitative differences between samples with different Ni/Zr ratio.

Nanofocusing, high-resolution X-ray optics demand good surface quality, the absence of tapered sidewalls, and a depth reaching into tens, sometimes hundreds of microns, all requirements that must be satisfied over large areas. In this report, we discuss our motivation for choosing group IV materials (predominantly Si, and C in its diamond form) for nanofocusing and high resolution in the hard X-ray portion of the spectrum. We elaborate on the design and nanofabrication procedures, and detail the etching parameters that offer a path for overcoming obstacles in making better optics. We briefly review tests for the assessing the quality of the optics.

We report a comparison of the room temperature recrystallization of electroplated (EP) copper in blanket films as a function of thickness measured by focused ion beam (FIB) microscope images and sheet resistance measurements. Both sets of data show an increase in rate with film thickness from 0.75νm up to 5νm, while little recrystallization is observed in films thinner than 0.75νm. Interestingly, the recrystallization rates from FIB analysis are consistently faster than those from the sheet resistance measurements. These data suggest that the recrystallization is initiated close to the top surface of the EP Cu film, but that in thinner films a high surface-to-volume ratio allows surface inhibition or pinning to retard the transformation. A Johnson-Mehl-AvramiKolmogorov (JMAK) analysis of the two data sets yields unusually high values for the Avrami exponent μ of up to 7 for the FIB data, while lower values of around 4 are obtained for the sheet resistance data. X-ray diffraction pole figures of the films have also been collected and correlations between the crystallographic texture, film thickness and recrystallization are discussed.

The microstructure of narrow metal conductors in the electrical interconnections on IC chips has often been identified as of major importance in the reliability of these devices. The stresses and stress gradients that develop in the conductors as a result of thermal expansion differences in the materials and of electromigration at high current densities are believed to be strongly dependent on the details of the grain structure. The present work discusses new techniques based on microbeam x-ray diffraction (MBXRD) that have enabled measurement not only of the microstructure of totally encapsulated conductors but also of the local stresses in them on a micron and submicron scale. White x-rays from the Advanced Light Source were focused to a micron spot size by Kirkpatrick-Baez mirrors. The sample was stepped under the micro-beam and Laue images obtained at each sample location using a CCD area detector. Microstructure and local strain were deduced from these images. Cu lines with widths ranging from 0.8 [.proportional]m to 5 [.proportional]m and thickness of 1 [.proportional]m were investigated. Comparisons are made between the capabilities of MBXRD and the well established techniques of broad beam XRD, electron back scatter diffraction (EBSD) and focused ion beam imagining (FIB).

The transistors planned for commercial use ten years from now in many electronic devices will have gate lengths shorter than 130 atoms, gate oxides thinner than 1.2 nm of SiO2 and clock speeds in excess of 10 GHz. It is now technologically possible to produce such transistors with gate oxides only 5 silicon atoms thick[l]. Since at least two of those 5 atoms are not in a local environment similar to either bulk Si or bulk SiO2, the properties of the interface are responsible for a significant fraction of the “bulk” properties of the gate oxide. However the physical (and especially their electrical) properties of the interfacial atoms are very different from .bulk Si or bulk SiO2. Further, roughness on an atomic scale can alter the leakage current by orders of magnitude.

In our studies of such devices, we found that thermal oxidation tends to produce Si/SiO2 interfaces with 0.1-0.2 nm rms roughness.

Electroplated Cu films undergo a remarkable recrystallization at room temperature that has been associated with dislocations and defects arising from the influence of surface-active additives during plating. In the process of plating, the composition of the bath changes as the organic additives are depleted by incorporation into the Cu films or electrolytic decomposition and replenished by fresh additions. Given the sensitivity of the plating process to low concentrations of additives, the properties of the plated Cu might be expected to differ between a freshly prepared bath and an older bath that has processed thousands of wafers and achieved a steady state composition of additives and by-products.

In this paper we compare the recrystallization rates of Cu films deposited from two such baths on wafers with damascene trenches of widths from 0.3 to 5 μm. Films deposited from the older bath consistently recrystallize at a faster rate for all trench widths and both barrier materials (Ta, TaN) studied. The concentration of impurities is comparable in the two films. Therefore, the difference in rates is likely due to a difference in defect densities in the film due to different adsorbate/surface interactions during plating. Although the recrystallization rates vary, X-ray diffraction pole figure analysis of films plated from the two baths show no differences in texture. Sidewall growth components are visible in both sets of samples. Data on the influence of the barrier material and trench width on recrystallization rates are also presented.

Electroplated Cu films undergo a remarkable recrystallization at room temperature that has been associated with dislocations and defects arising from the influence of surface-active additives during plating. In the process of plating, the composition of the bath changes as the organic additives are depleted by incorporation into the Cu films or electrolytic decomposition and replenished by fresh additions. Given the sensitivity of the plating process to low concentrations of additives, the properties of the plated Cu might be expected to differ between a freshly prepared bath and an older bath that has processed thousands of wafers and achieved a steady state composition of additives and by-products.

In this paper we compare the recrystallization rates of Cu films deposited from two such baths on wafers with damascene trenches of widths from 0.3 to 5 μm. Films deposited from the older bath consistently recrystallize at a faster rate for all trench widths and both barrier materials (Ta, TaN) studied. The concentration of impurities is comparable in the two films. Therefore, the difference in rates is likely due to a difference in defect densities in the film due to different adsorbate/surface interactions during plating. Although the recrystallization rates vary, X-ray diffraction pole figure analysis of films plated from the two baths show no differences in texture. Sidewall growth components are visible in both sets of samples. Data on the influence of the barrier material and trench width on recrystallization rates are also presented.

As interconnect technology moves deeper into the submicron realm, the physics governing the mechanical behavior, hence the reliability of metal lines changes. Events at the level of individual grains become more important. One would like to be able to measure the strain and orientation of single grains, and the distribution of strain across a grain. Such data may help us understand such effects as sunken grains, the erratic occurrence of stress voiding and Blechlength effects in electromigration. To get this information, techniques involving X-ray diffraction with submicron beams are being developed. These experiments involve detecting Laue spots from selected areas and energy-analyzing them to find the strain tensor. Motivations for such measurements, the specifications for a useful instrument, some designs now being developed and the intrinsic limitations of these approaches will be discussed. Design issues in the choice of focussing optics and energy measurement will be highlighted with calculations of how the Laue spots would look for different conditions of crystal perfection.

Root mean square measurements of the Si(001)/SiO2 interface have been performed with a variety of techniques. Using X-ray diffraction to represent the diffraction class of techniques, and atomic force microscopy to represent imaging techniques, we discuss the effect that limitations of each technique have on experimental results.