In OperandoGISAXS Studies of Mound Coarsening in Electrochemical Homoepitaxy

Abstract

Kinetic roughening during electrodeposition was studied by grazing incidence small angle x-ray scattering for the case of Au(001) homoepitaxial growth in Cl- containing electrolytes. The formation and coarsening of an isotropic mound distribution on unreconstructed Au(001) and of [110]-oriented anisotropic mounds on the "hex" reconstructed surface was observed. The lateral mound coarsening is described by a well-defined scaling law. On unreconstructed Au a transition in the coarsening exponent from ≈1/4 to ≈1/3 with increasing potential is found, which can be explained by the pronounced potential dependence of surface transport processes in an electrochemical environment.

Advanced grazing-incidence techniques for modern soft-matter materials analysis

“…In particular, in operando studies of energy-related materials are receiving increasing attention, although frequently addressing hard condensed matter. For example, for the case of Au(001) homoepitaxial growth in Cl-containing electrolytes, the kinetics of roughening were studied with in operando GISAXS during electrodeposition (Ruge et al, 2014). An example from soft matter deals with proton-conducting ionomers.…”

Diffusion and nucleation in multilayer growth of PTCDI-C8 studied with in situ X-ray growth oscillations and real-time small angle X-ray scattering

“…It has been shown that the temporal evolution of island densities can even be examined in situ during the film growth by applying grazing-incidence small-angle X-ray scattering (GISAXS). [9][10][11][12][13] In addition, the evolution of the out-of-plane structure can be simultaneously monitored by specular Xray reflectivity (XRR) during the growth of thin-films. In numerous studies, non-invasive in situ and real-time XRR has been successfully used for analyzing the growth of organic systems.…”

Using GISAXS to Detect Correlations between the Locations of Gold Particles Electrodeposited from an Aqueous Solution

“…examined the dissolution of a gold (100) surface in a chloride containing solution 33 and Magnussen et al reported the surface dynamics of gold deposited on a gold (100) surface. 34,35 In this work, we have used GISAXS to investigate the electrodeposition of gold from an aqueous solution on TiN, a widely used material in microelectronics and an increasingly popular electrode material. 36 The study of Au electrodeposition has been mainly addressed in the past using glassy carbon or n-Si electrodes, 19,[37][38][39] We show that even though electron microscopy is very useful as a characterization method for these systems, the use of GISAXS allows for the detection of non-random order within a seemingly disordered arrangement of particles, proving that nucleation during electrodeposition of Au on TiN is not a fully random process.…”

“…31, 32 Golks et al examined the dissolution of a gold (100) surface in a chloride-containing solution 33 and Magnussen et al reported the surface dynamics of gold deposited on a gold (100) surface. 34,35 In this work, we have used GISAXS to investigate the electrodeposition of gold from an aqueous solution on TiN, a widely used material in microelectronics and an increasingly popular electrode material. 36 The study of Au electrodeposition has been mainly addressed in the past using glassy carbon or n-Si electrodes.…”

“…GISAXS has been used recently for the in situ investigation of sputter deposition on different inorganic and organic substrates and for spray deposition of various materials, where the formation of the deposited materials was followed in real time. − ,− For electrochemical systems, only a handful of studies using X-rays (both transmission SAXS, GISAXS, and surface X-ray powder diffraction (XRD)) can be found in the literature. Ustarroz et al looked at the deposition of silver nanoparticles on carbon using SAXS. , Golks et al examined the dissolution of a gold (100) surface in a chloride-containing solution and Magnussen et al reported the surface dynamics of gold deposited on a gold (100) surface. , …”