In-Situ X-ray Photoemission Spectromicroscopy of Electromigration in Patterned Al-Cu Lines With Maximum

1998 ◽  
Vol 516 ◽  
Author(s):  
H.H. Solak ◽  
G.F. Lorusso ◽  
S. Singh ◽  
F. Cerrina ◽  
J.H. Underwood ◽  
...  
Keyword(s):  
Spectral Region ◽  
Structural Changes ◽  
Region Of Interest ◽  
Sample Surface ◽  
X Rays ◽  
Energy Analyzer ◽  
X Ray ◽  
Before And After ◽  
Chemical States

AbstractWe report the application of a unique photoemission spectromicroscope (MAXIMUM) to the study of electromigration phenomena in Al-Cu interconnects. MAXIMUM is a scanning type photoemission microscope that uses multilayer-coated optics to focus 130 eV x-rays to a sub-0.1 µm spot. An electron energy analyzer collects photoelectrons in a chosen spectral region of interest to form an image of the sample that is sensitive to chemical states of elements on the sample surface. Al-Cu lines were characterized by spectromicroscopy techniques before and after electromigration stressing in the UHV environment of the microscope chamber. We present spectro-micrographs showing the chemical and structural changes on Al-Cu line surfaces as a result of the electromigration process.

In Situ Monitoring of the Electrochemical Absorption of Deuterium into Palladium by X-Ray Diffraction using Synchrotron-Wiggler Radiation

1998 ◽  
Vol 524 ◽  
Author(s):  
D. D. Dominguez ◽  
P. L. Hagans ◽  
E. F. Skelton ◽  
S. B. Qadri ◽  
D. J. Nagel
Keyword(s):  
Structural Changes ◽  
National Laboratory ◽  
High Energy ◽  
Brookhaven National Laboratory ◽  
In Situ Monitoring ◽  
X Rays ◽  
X Ray ◽  
Β Phase ◽  
Metallic Sample

ABSTRACTWith 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.

scholarly journals In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays: High Resolution Imaging at Ambient Pressure and Elevated Temperature

2016 ◽  
Vol 22 (1) ◽  
pp. 178-188 ◽  
Author(s):  
Sina Baier ◽  
Christian D. Damsgaard ◽  
Maria Scholz ◽  
Federico Benzi ◽  
Amélie Rochet ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Elevated Temperature ◽  
Gas Flow ◽  
Heterogeneous Catalysts ◽  
Ambient Pressure ◽  
Ex Situ ◽  
X Rays ◽  
X Ray ◽  
Before And After

AbstractA new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin electron transparent window and allows heating. Two gold-based systems, 50 nm gold particles and nanoporous gold as a relevant catalyst sample, were used for studying the feasibility of the cell. Measurements showing a resolution around 40 nm have been achieved under a flow of synthetic air and during heating up to temperatures of 933 K. An elevated temperature exhibited little influence on image quality and resolution. With this study, the potential of in situ hard X-ray ptychography for investigating annealing processes of real catalyst samples is demonstrated. Furthermore, the possibility to use the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample.

scholarly journals Angular-split/temporal-delay approach to ultrafast protein dynamics at XFELs

2016 ◽  
Vol 72 (7) ◽  
pp. 871-882 ◽  
Author(s):  
Zhong Ren ◽  
Xiaojing Yang
Keyword(s):  
Structural Changes ◽  
Ultrashort Pulses ◽  
Atomic Displacement ◽  
Atomic Resolution ◽  
Biological Macromolecules ◽  
X Rays ◽  
Temporal Delay ◽  
X Ray ◽  
X Ray Crystallography ◽  
Before And After

X-ray crystallography promises direct insights into electron-density changes that lead to and arise from structural changes such as electron and proton transfer and the formation, rupture and isomerization of chemical bonds. The ultrashort pulses of hard X-rays produced by free-electron lasers present an exciting opportunity for capturing ultrafast structural events in biological macromolecules within femtoseconds after photoexcitation. However, shot-to-shot fluctuations, which are inherent to the very process of self-amplified spontaneous emission (SASE) that generates the ultrashort X-ray pulses, are a major source of noise that may conceal signals from structural changes. Here, a new approach is proposed to angularly split a single SASE pulse and to produce a temporal delay of picoseconds between the split pulses. These split pulses will allow the probing of two distinct states before and after photoexcitation triggered by a laser pulse between the split X-ray pulses. The split pulses originate from a single SASE pulse and share many common properties; thus, noise arising from shot-to-shot fluctuations is self-canceling. The unambiguous interpretation of ultrafast structural changes would require diffraction data at atomic resolution, as these changes may or may not involve any atomic displacement. This approach, in combination with the strategy of serial crystallography, offers a solution to study ultrafast dynamics of light-initiated biochemical reactions or biological processes at atomic resolution.

The Basic Physical Principles of Ion, Electron, and X-Ray Detectors and Their Application to Microanalysis

1985 ◽  
Vol 43 ◽  
pp. 154-157
Author(s):  
A.J. Tousimis
Keyword(s):  
Ion Beam ◽  
Depth Resolution ◽  
Sample Surface ◽  
High Energy ◽  
X Rays ◽  
X Ray ◽  
Electrons And Ions ◽  
Spatial Depth ◽  
Minimum Surface Area ◽  
Physical Principles

An integral and of prime importance of any microtopography and microanalysis instrument system is its electron, x-ray and ion detector(s). The resolution and sensitivity of the electron microscope (TEM, SEM, STEM) and microanalyzers (SIMS and electron probe x-ray microanalyzers) are closely related to those of the sensing and recording devices incorporated with them.Table I lists characteristic sensitivities, minimum surface area and depth analyzed by various methods. Smaller ion, electron and x-ray beam diameters than those listed, are possible with currently available electromagnetic or electrostatic columns. Therefore, improvements in sensitivity and spatial/depth resolution of microanalysis will follow that of the detectors. In most of these methods, the sample surface is subjected to a stationary, line or raster scanning photon, electron or ion beam. The resultant radiation: photons (low energy) or high energy (x-rays), electrons and ions are detected and analyzed.

scholarly journals Physical and chemical imaging of adhesive interfaces with soft X-rays

2021 ◽  
Vol 2 (1) ◽  
Author(s):  
Hiroyuki Yamane ◽  
Masaki Oura ◽  
Osamu Takahashi ◽  
Tomoko Ishihara ◽  
Noriko Yamazaki ◽  
...  
Keyword(s):  
Molecular Level ◽  
Covalent Bond ◽  
Chemical Imaging ◽  
Diglycidyl Ether ◽  
X Rays ◽  
X Ray ◽  
Covalent Bond Formation ◽  
Chemical States ◽  
The Individual ◽  
Physical And Chemical

AbstractAdhesion is an interfacial phenomenon that is critical for assembling carbon structural composites for next-generation aircraft and automobiles. However, there is limited understanding of adhesion on the molecular level because of the difficulty in revealing the individual bonding factors. Here, using soft X-ray spectromicroscopy we show the physical and chemical states of an adhesive interface composed of a thermosetting polymer of 4,4’-diaminodiphenylsulfone-cured bisphenol A diglycidyl ether adhered to a thermoplastic polymer of plasma-treated polyetheretherketone. We observe multiscale phenomena in the adhesion mechanisms, including sub-mm complex interface structure, sub-μm distribution of the functional groups, and molecular-level covalent-bond formation. These results provide a benchmark for further research to examine how physical and chemical states correlate with adhesion, and demonstrate that soft X-ray imaging is a promising approach for visualizing the physical and chemical states at adhesive interfaces from the sub-mm level to the molecular level.

scholarly journals High temperature structural study of decagonal Al-Cu-Rh quasicrystal.

2014 ◽  
Vol 70 (a1) ◽  
pp. C94-C94
Author(s):  
Pawel Kuczera ◽  
Walter Steurer
Keyword(s):  
Structural Changes ◽  
Configurational Entropy ◽  
Lattice Vibrations ◽  
X Ray Diffraction ◽  
Stabilization Mechanism ◽  
X Ray ◽  
Comparative Structure ◽  
The Stability

The structure of d(ecagonal)-Al-Cu-Rh has been studied as a function of temperature by in-situ single-crystal X-ray diffraction in order to contribute to the discussion on energy or entropy stabilization of quasicrystals (QC) [1]. The experiments were performed at 293 K, 1223 K, 1153 K, 1083 K, and 1013 K. A common subset of 1460 unique reflections was used for the comparative structure refinements at each temperature. The results obtained for the HT structure refinements of d-Al-Cu-Rh QC seem to contradict a pure phasonic-entropy-based stabilization mechanism [2] for this QC. The trends observed for the ln func(I(T1 )/I(T2 )) vs.|k⊥ |^2 plots indicate that the best on-average quasiperiodic order exists between 1083 K and 1153 K, however, what that actually means is unclear. It could indicate towards a small phasonic contribution to entropy, but such contribution is not seen in the structure refinements. A rough estimation of the hypothetic phason instability temperature shows that it would be kinetically inaccessible and thus the phase transition to a 12 Å low T structure (at ~800 K) is most likely not phason-driven. Except for the obvious increase in the amplitude of the thermal motion, no other significant structural changes, in particular no sources of additional phason-related configurational entropy, were found. All structures are refined to very similar R-values, which proves that the quality of the refinement at each temperature is the same. This suggests, that concerning the stability factors, some QCs could be similar to other HT complex intermetallic phases. The experimental results clearly show that at least the ~4 Å structure of d-Al-Cu-Rh is a HT phase therefore entropy plays an important role in its stabilisation mechanism lowering the free energy. However, the main source of this entropy is probably not related to phason flips, but rather to lattice vibrations, occupational disorder unrelated to phason flips like split positions along the periodic axis.

In Situ Testing and X Rays Radiation Effects of Pt/Bi3.15Nd0.85Ti3O12/Pt Ferroelectric Capacitors

2013 ◽  
Vol 712-715 ◽  
pp. 293-297
Author(s):  
Li Li
Keyword(s):  
Radiation Effects ◽  
Hysteresis Loops ◽  
Electrical Performance ◽  
Hysteresis Curve ◽  
X Rays ◽  
Shanghai Synchrotron Radiation Facility ◽  
X Ray ◽  
In The Beginning ◽  
Ferroelectric Capacitors

Pt/Bi3.15Nd0.85Ti3O12(BNT)/Pt ferroelectric capacitors were monitored using in situ X-ray irradiation with 10 keV at BL14B1 beamline (Shanghai Synchrotron Radiation Facility). BL14B1 combined with a ferroelectric analyzer enabled measurements in situ of electrical performance. The hysteresis curve (PE) of distortion depended on the polarization during irradiation, but the diffracted intensities of the (117) peak did not change in the beginning. ThePEcurve had a negligible change from 2.09×109Gy to 4.45×109Gy. Finally, bothPrandPr+very rapidly increased, but the intensities of (117) decreased. The hysteresis loops were remarkably deformed at the maximum total dose of 4.87×109Gy.

Applications of High-Resolution Powder X-Ray Diffraction

2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch
Keyword(s):  
High Resolution ◽  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Characterisation ◽  
Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

scholarly journals In Situ Coherent X-ray Diffraction during Three-Point Bending of a Au Nanowire: Visualization and Quantification

2018 ◽  
Vol 2 (4) ◽  
pp. 24 ◽  
Author(s):  
Anton Davydok ◽  
Thomas Cornelius ◽  
Zhe Ren ◽  
Cedric Leclere ◽  
Gilbert Chahine ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Reciprocal Space ◽  
X Ray Diffraction ◽  
Complex Deformation ◽  
X Ray ◽  
Three Point Bending ◽  
Atomic Force ◽  
Au Nanowire ◽  
Before And After

The three-point bending behavior of a single Au nanowire deformed by an atomic force microscope was monitored by coherent X-ray diffraction using a sub-micrometer sized hard X-ray beam. Three-dimensional reciprocal-space maps were recorded before and after deformation by standard rocking curves and were measured by scanning the energy of the incident X-ray beam during deformation at different loading stages. The mechanical behavior of the nanowire was visualized in reciprocal space and a complex deformation mechanism is described. In addition to the expected bending of the nanowire, torsion was detected. Bending and torsion angles were quantified from the high-resolution diffraction data.

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