With low energy x-rays, such as those from a Cu x-ray tube, only the outer few microns of a metallic sample can be probed. This low penetrating power prohibits structural studies from being carried out on the interior of an electrode in an electrochemical cell because of absorption by the cell material, electrodes and the electrolyte. The work described in this paper circumvents this problem by utilizing high energy, high brightness x-rays produced on the superconducting wiggler beam line, X-17C, at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory. The penetrating power of the higher energy x-rays allowed Pd diffraction spectra to be obtained in-situ on a 1 mm diameter Pd wire cathode during electrolysis of heavy water. Moreover, the beam (28 × 28 μm in cross-section) allowed diffraction spectra to be acquired as a function of distance across the sample. Spectra were recorded in 50 μm steps from the edge of the Pd wire to its core. This was done at 2 minute intervals as a function of electrolysis time. The α-β phase transition induced in the Pd while deuterium was electrochemically absorbed was observed by monitoring the Pd-(422) diffraction peaks. Results allowed the diffusion rate and the diffusivity of deuterium atoms in the Pd wire to be determined. Other features of the structural changes associated with the absorption of deuterium into Pd are reported.

High pressure synchrotron x-ray diffraction experiments were conducted on KCa2Nb3O10, to determine lattice constants as a function of pressure. A diamond anvil cell was used to produce pressures up to 66 GPa. A phase transition occurred at 13.5 GPa. From the lattice constants, linear compressibilities of 8.55 × 10-4 GPa-1 in the a direction, -9.40 × 10-4 GPa-1 in the b direction, and 142 × 10-4 GPa-1 in the c direction, and a bulk modulus of 68.5 GPa were found for the lower pressure orthorhombic phase.

A compact tube furnace has been developed for high temperature X-ray diffraction studies using high energy synchrotron radiation. The furnace design has a low absorption path in transmission yet allows for a high degree of control of the sample atmosphere and a minimal temperature gradient across the sample. The design allows for a maximum temperature of 1500°C with a variety of atmospheres including inert, reducing, and oxidizing. Preliminary results obtained at the SRI-CAT I-ID undulator line (60keV) at the APS facility and the A2 24 pole wiggler line (45keV) at CHESS on the Ti5Si3Z5 (Z = C, N, O) system will be presented to demonstrate the feasibility of this approach.

Interfacial structure and the atomic interactions between atoms at interfaces in multilayers or nano-laminates have significant impact on the physical properties of these materials. A technique for the experimental evaluation of interfacial structure and interfacial structure effects is presented and compared to experiment. In this paper the impact of interfacial structure on the performance of x-ray, soft x-ray and extreme ultra-violet multilayer optic structures is emphasized. The paper is concluded with summary of these results and an assessment of their implications relative to multilayer development and the study of buried interfaces in solids in general.

The minimum-detectable-limit of a compact double-focusing graphite mosaic-crystal spectrometer is compared to the minimum-detectable-limit from a high-performance Ge solidstate detector. The solid angle and efficiency of the solid-state detector is much greater than for the crystal spectrometer. However, the better signal-to-noise of the spectrometer and its insensitivity to matrix fluorescence and scattering can give it a better minimum-detectable-limit for trace element analysis. The relative advantages of the two detectors are illustrated for some simple test samples. The performance of the crystal spectrometer compared to the solid-state detector increases as the flux in the x-ray probe increases. This makes crystal spectrometers especially interesting for use with new high intensity 3rd generation synchrotron microprobes. An estimate is made of the source and sample conditions favored for each detector.

Bragg reflection (001) of high-quality crystal of ammonium acid phthalate (2d = 52.28 A˚) is investigated in the region of CK absorption edge. First order reflection for this crystal is forbidden. Due to anisotropic additions, it appears only near CK edge. Two-crystal optical scheme was used for the measurement of the crystal reflectivity. As shown, the change of crystal azimuth in X-ray spectrometer leads to ability to control the resolution. Rotation effects of X-ray beam polarization on 90° angle is considered for the forbidden reflection.

Performance of future generations of integrated circuits will be limited by the RC delay caused by on-chip interconnections. Overcoming this limitation requires the deployment of new high conductivity metals such as copper and low dielectric constant intermetal dielectrics (IMD). Fluorinated amorphous carbon (a-CFx) is a promising candidate for replacing SiO2 as the IMD. In this paper we investigated the structure and electronic properties of a-CFx thin films using high-resolution x-ray absorption, emission, and photoelectron spectroscopy. The composition and local bonding information were obtained and correlated with deposition conditions. The data suggest that the structure of the a-CFx is mostly of carbon rings and CF2 chains cross-linked with C atoms. The effects of growth temperature on the structure and the thermal stability of the film are discussed.

In this work, in-situ doped polysilicon and poly-SiGe films have been used as the gate material for the fabrication of MOS devices to evaluate their respective performances. These films were deposited in an RTCVD system using a Si2H6 and GeH4 gas mixture. MOS capacitors with 45 Å thick gate oxides and polysilicon/poly-SiGe gates were subjected to different anneals to study boron penetration. SIMS analysis and flat band voltage measurements showed much lower boron penetration for devices with poly-SiGe gates than for devices with polysilicon gates. In addition, C-V measurements showed no poly depletion effects for poly-SiGe gates while polysilicon gates had a depletion effect of about 8%. A comparison of resistivities of these films showed a low resistivity of 1 mΩ-cm for poly-SiGe films versus 3 mΩ-cm for polysilicon films after an anneal at 950 °C for 30 seconds.

The first preliminary results from a novel spectrometer for elementally-specific measurements of magnetic surfaces and ultrathin films are presented here. The key measurements are based upon spin-resolving and photon-dichroic photoelectron spectroscopy. True spinresolution is achieved by the use of a Mini-Mott detection scheme. The photon-dichroic measurements include the variant magnetic x-ray linear dichroism (MXLD). Both a multi-channel, energy dispersive collection scheme as well as the spin-detecting Mini-Mott apparatus are used in data collection. The [Spin Spectrometer] is based at the Spectromicroscopy Facility (Beamline7)at the Advanced Light Source.

The magnetic properties of strained thin films of gadolinium are characterized by a wave vector and thickness dependence of the exchange splitting. The spin-resolved band structure has been mapped by spin polarized photoemission, and provides considerable insight into the relationship between magnetism of local moment systems, and band structure.

The constructive interference between direct and indirect channels above the absorption threshold of a core level leads to a massive increase in the emission cross section leading to a phenomenon called “resonant photoemission”. Using novel magnetic linear dichroism in angular distribution photoelectron spectroscopy experiment we have tried to understand the nature of the resonant photoemission process in Gd metal. The presence of dichroism in Gd 4f photoemission intensity at a photon energy corresponding to resonant photoemission clearly demonstrates the photoemission-like nature of the resonant photoemission process.

The chemical sensitivity, spatial resolution and data acquisition rates achieved with the scanning photoelectron microscope built at ELETTRA, a third-generation synchrotron facility in Italy has made it an indispensable tool for surface analysis of laterally heterogeneous materials. The information on the composition and evolution of coexisting phases, mass transport and other surface processes occurring on a microscopic scale can be obtained by combining elemental and chemical mapping with core and valence level photoelectron spectromicroscopy with spatial resolution better than 0.15 μm and energy resolution better than 0.5 eV. Selected recent results will be presented to illustrate the capabilities and some of the possible applications of synchrotron radiation spectromicroscopy for characterization of complex spatially heterogeneous materials and studies of dynamic processes related to the interface chemical structure.

We present recent results obtained by MAXIMUM at the Advanced Light Source (ALS), at the Lawrence Berkeley National Laboratory. MAXIMUM is a scanning photoemission microscope, based on a multilayer coated Schwarzschild objective. An electron energy analyzer collects the emitted photoelectrons to form an image as the sample itself is scanned. The microscope has been purposely designed to take advantage of the high brightness of the third generation synchrotron radiation sources, and it installation at ALS has been recently completed. The spatial resolution of 100 nm and the spectral resolution of 200 meV make our instrument an extremely interesting tool to investigate current problems in opto- and microelectronics. In order to illustrate the potential of MAXIMUM in these fields, we report new results obtained by studying the electromigration in Al-Cu lines and the Al segregation in AIGaN thin films.

This paper presents preliminary data on analyses of selected materials using two state-ofthe- art XPS systems: the Physical Electronics Inc. (PHI, Eden Prairie, MN) Quantum 2000 instrument and the microXPS beamline (7.3.2.1) at the Advanced Light Source (ALS). This research compares and contrasts relevant performance characteristics of the two systems including elemental and chemical state detection sensitivity, imaging capabilities including lateral resolution and useful image fields, role of X-ray dose damage to surface, analysis speed as well as analytical throughput.

Chemical analysis on a microscopic scale was performed on a TiN particle sample on silicon and on two patterned samples using a synchrotron source scanning photoemission microscope. For all the experiments, we exploit the ability, developed in our experimental system, to reach specific locations on the wafer and analyze the local chemical state.

TRISO fuel particles contain a small kernel of nuclear fuel encapsulated by alternating layers of C and a barrier layer of SiC. The TRISO fuel particle is used in an advanced nuclear fuel where the SiC shell provides the primary barrier for radioactive elements in the kernel. The performance of this barrier is key to containment. We have used x-ray fluorescence microtomography to measure the trace element distribution in a SiC shell. Prior to our measurements the nuclear fuel and C layers were leached from the particle. The shell was then encapsulated by kapton tape to simplify handling. The shell was mounted on a glass fiber and measurements were made with an ∼1 x3 ωm2 x-ray probe on beamline 2-ID at the APS. The distribution of trace elements in the SIC shell was reconstructed after correcting the data for artifacts arising from absorption and scattering off the kapton tape. The observed trace elements are distributed in small <1ωm regions through the SiC shell. The trace elements can be attributed to radiation enhanced diffusion of elements in the kernel or to trace elements introduced during fabrication. X-ray fluorescence microtomography is an ideal tool for this work because it is a penetrating nondestructive probe sensitive to trace elements in a low Z matrix and because it provides a picture of the elemental distribution in the shell.

Synchrotron x-ray fluorescence microscopy has been used to study multi-metal oxide ceramics that have been designed to sequester radioactive actinide elements for long-term storage and disposal. X-ray fluorescent lines for the various elements have been used for lateral elemental mapping of the materials, and the heterogeneity of the samples is discussed with respect to the elements in the crystallographic phases that have previously been documented by other means of structural and chemical analyses.

Synchrotron-based total-reflection x-ray fluorescence(SR-TXRF) has been developed as a leading technique for measuring wafer cleanliness. It holds advantages over other techniques in that it is non-destructive and allows mapping of the surface. The highest sensitivity observed thus far is 3x108 atoms/cm 2 (- 3fg) for 1000 second count time. Several applications of SR-TXRF are presented which take advantage of the energy tunability of the synchrotron source or the mapping capability.

X-ray absorption measurements are described for identifying metal impurities insilica preforms, the rod-like starting materials from which hair-like optical fibers are drawn.The results demonstrate the effectiveness of this approach as a non-destructive,quantitative, element-selective, position-sensitive, and chemical-state-specific means forcharacterizing transition metals in the concentration regime of parts per billion.

We present the formalism of anomalous x-ray scattering as applied to partial structure analysis of disordered materials, and give an example of how the technique has been applied, together with that of neutron diffraction, to investigate short-, intermediate- and extended-range order in vitreous germania and rubidium germanate.