A refraction correction for buried interfaces applied to in situ grazing-incidence X-ray diffraction studies on Pd electrodes

In situ characterization of electrochemical systems can provide deep insights into the structure of electrodes under applied potential. Grazing-incidence X-ray diffraction (GIXRD) is a particularly valuable tool owing to its ability to characterize the near-surface structure of electrodes through a layer of electrolyte, which is of paramount importance in surface-mediated processes such as catalysis and adsorption. Corrections for the refraction that occurs as an X-ray passes through an interface have been derived for a vacuum–material interface. In this work, a more general form of the refraction correction was developed which can be applied to buried interfaces, including liquid–solid interfaces. The correction is largest at incidence angles near the critical angle for the interface and decreases at angles larger and smaller than the critical angle. Effective optical constants are also introduced which can be used to calculate the critical angle for total external reflection at the interface. This correction is applied to GIXRD measurements of an aqueous electrolyte–Pd interface, demonstrating that the correction allows for the comparison of GIXRD measurements at multiple incidence angles. This work improves quantitative analysis of d-spacing values from GIXRD measurements of liquid–solid systems, facilitating the connection between electrochemical behavior and structure under in situ conditions.

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X-RAY DIFFRACTION FOR SURFACES AND BURIED INTERFACES

Surface Review and Letters ◽

10.1142/s0218625x00000452 ◽

2000 ◽

Vol 07 (04) ◽

pp. 437-446 ◽

Cited By ~ 1

Author(s):

G. RENAUD

Keyword(s):

Grazing Incidence ◽

X Rays ◽

X Ray Diffraction ◽

X Ray ◽

Grain Sizes ◽

Buried Interfaces ◽

Surfaces And Interfaces ◽

Coherent Interfaces

The application of X-rays to the structural characterization of surfaces and interfaces, in situ and in UHV, is discussed on selected examples. Grazing incidence X-ray diffraction is not only a very powerful technique for quantitatively investigating the atomic structure of surfaces and interfaces, but is also very useful for providing information on the interfacial registry for coherent interfaces or on the strain deformation, island and grain sizes for incoherent epilayers.

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A flow cell for transient voltammetry and in situ grazing incidence X-ray diffraction characterization of electrocrystallized cadmium(II) tetracyanoquinodimethane

Electrochimica Acta ◽

10.1016/j.electacta.2010.09.106 ◽

2011 ◽

Vol 56 (3) ◽

pp. 1546-1553 ◽

Cited By ~ 8

Author(s):

Jean-Pierre Veder ◽

Ayman Nafady ◽

Graeme Clarke ◽

Ross P. Williams ◽

Roland De Marco ◽

...

Keyword(s):

Grazing Incidence ◽

Flow Cell ◽

X Ray Diffraction ◽

X Ray

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In situ electrochemical impedance spectroscopy/synchrotron radiation grazing incidence X-ray diffraction—A powerful new technique for the characterization of electrochemical surfaces and interfaces

Electrochimica Acta ◽

10.1016/j.electacta.2006.03.030 ◽

2006 ◽

Vol 51 (26) ◽

pp. 5920-5925 ◽

Cited By ~ 15

Author(s):

Roland De Marco ◽

Zhong-Tao Jiang ◽

Jay Martizano ◽

Alex Lowe ◽

Bobby Pejcic ◽

...

Keyword(s):

Electrochemical Impedance Spectroscopy ◽

Synchrotron Radiation ◽

Impedance Spectroscopy ◽

Electrochemical Impedance ◽

Grazing Incidence ◽

X Ray Diffraction ◽

X Ray ◽

Surfaces And Interfaces

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Growth mechanisms of Pd nanofilms electrodeposited onto Au(111): an in situ grazing incidence X-ray diffraction study

Physical Chemistry Chemical Physics ◽

10.1039/c5cp05985b ◽

2016 ◽

Vol 18 (4) ◽

pp. 2830-2839 ◽

Cited By ~ 5

Author(s):

Yvonne Soldo-Olivier ◽

Maurizio De Santis ◽

Wang Liang ◽

Eric Sibert

Keyword(s):

Diffraction Study ◽

Grazing Incidence ◽

Growth Mechanisms ◽

X Ray Diffraction ◽

X Ray

Surface X-ray diffraction characterization of a Pd10ML/Au(111) film. A characteristic Pd rod with sharp Bragg-like peaks is observed, signature of 3D islands growth.

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In situ synchrotron radiation grazing incidence X-ray diffraction—A powerful technique for the characterization of solid-state ion-selective electrode surfaces

Electrochimica Acta ◽

10.1016/j.electacta.2006.01.034 ◽

2006 ◽

Vol 51 (23) ◽

pp. 4886-4891 ◽

Cited By ~ 11

Author(s):

Roland De Marco ◽

Zhong-Tao Jiang ◽

Bobby Pejcic ◽

Arie van Riessen

Keyword(s):

Solid State ◽

Synchrotron Radiation ◽

Grazing Incidence ◽

X Ray Diffraction ◽

Selective Electrode ◽

X Ray ◽

Powerful Technique ◽

Electrode Surfaces

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In situ Characterization Of MBE Grown Surfaces And Interfaces By Grazing Incidence X-Ray Diffraction

10.1117/12.963911 ◽

1990 ◽

Author(s):

R. Pinchaux ◽

M. Sauvage-Simkin ◽

J. Massies ◽

N. Jedrecy ◽

N. Greiser ◽

...

Keyword(s):

Grazing Incidence ◽

X Ray Diffraction ◽

In Situ Characterization ◽

X Ray ◽

Surfaces And Interfaces

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Structural Characterization of Multilayers Using X-ray Diffraction

MRS Proceedings ◽

10.1557/proc-239-475 ◽

1991 ◽

Vol 239 ◽

Cited By ~ 2

Author(s):

B. M. Clemens ◽

J-A. Bain ◽

A. P. Payne ◽

T. C. Hufnagel ◽

S. M. Brennan

Keyword(s):

Grazing Incidence ◽

Sputter Deposition ◽

X Ray Diffraction ◽

Deposition Pressure ◽

X Ray ◽

X Ray Scattering ◽

Multilayered Materials ◽

Cr System

ABSTRACTStructural deviations from ideal layering of bulk constituents can have dramatic effects on the properties of multilayered materials. We discuss three examples of the use of x-ray diffraction in non-standard geometries to examine these effects. In Mo/Ni multilayers, we use asymmetric diffraction and grazing incidence x-ray scattering (GIXS) to deduce the strain and intermixing. We find that coherency stresses between the BCC Mo and FCC Ni planes play a major role. In the Fe/Cr system, we use rocking curves and asymmetric scans about the small angle superlattice lines to investigate the nature and extent of layer roughness. We find that conformai roughness dominates our best samples, while non-conformal roughness increases with sputter deposition pressure. In the Gd/Co system, we use in-situ GIXS to investigate amorphization reaction during deposition. We find a strong diffusional asymmetry and rapid reaction during growth.

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The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100071107 ◽

1973 ◽

Vol 31 ◽

pp. 132-133 ◽

Cited By ~ 1

Author(s):

R. E. Herfert

Keyword(s):

Surface Characterization ◽

Analytical Techniques ◽

X Ray Diffraction ◽

Depth Of Penetration ◽

X Ray ◽

The Past ◽

Transmission Electron ◽

Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

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