Wen-Li Tsai

Electrochemistry: building on bubbles in metal electrodeposition.

In the electrodeposition of metals, a widely used industrial technique, bubbles of gas generated near the cathode can adversely affect the quality of the metal coating. Here we use phase-contrast radiology with synchrotron radiation to witness directly and in real time the accumulation of zinc on hydrogen bubbles. This process explains the origin of the bubble-shaped defects that are common in electrodeposited coatings.

Coherence-enhanced synchrotron radiology: simple theory and practical applications

The advanced characteristics of synchrotron x-ray sources make it possible to implement radiology with powerful and innovative approaches. We review in simple terms the conceptual background of such approaches, then we present a number of selected examples. The practical tests concern life-sciences specimens as well as materials-science systems.

Synchrotron X-ray induced solution precipitation of nanoparticles

Abstract By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100–300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (eaq−), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

pH dependence of synchrotron x-ray induced electroless nickel deposition

We investigated the room temperature electroless nickel deposition on glass, induced by synchrotron x ray. By irradiating electrolytes with intense x ray the onset time for Ni reduction disappears at high electrolyte pH (>6.0) in sharp contrast with conventional electroless deposition. The time for Ni reduction in irradiated solution also decreases with increase in electrolyte pH. Consequently higher reduction rates in alkaline solutions (pH>8.0) raise the Ni nucleation density during deposition, as illustrated by homogeneous and complete coverage of the substrate by nanoparticles within a short period of 1 min. The enhancement in reduction rate is attributed to high redox efficiency of hydrated electrons produced by x ray as well as their redox potential enhancements under higher electrolyte pH conditions.

Synchrotron radiographic study and computer simulation of reactions between micropipes in silicon carbide

By using synchrotron radiation phase sensitive radiography we have examined the reactions of screw superdislocations or micropipes in silicon carbide single crystals: bundling, twisting, and splitting. To understand the nature of these reactions, a model of micropipe motion during crystal growth has been proposed. Based on this model, a computer simulation of the evolution of a random micropipe ensemble has been performed. The simulation demonstrates that the coalescence of micropipes with opposite-sign Burgers vectors may be realized in two ways: (i) their straightforward movement towards each other or (ii) their revolution about one another. Twisted dislocation dipoles arise when two micropipes are under strong influence of the stress fields from dense groups of other micropipes. The transformation of dipoles into semiloops as well as the annihilation of micropipes result in diminishing of their average density

Ramification of micropipes in SiC crystals

The ramification of micropipes is observed using scanning electron microscopy, optical microscopy, and synchrotron x-ray radiography. The conditions for the ramification of dislocated micropipes are determined theoretically within a model when the angles between dislocation lines are small. It is shown that the ramification of micropipes into two smaller ones is possible only for micropipes with radii that exceed the equilibrium micropipe radius and is associated with a decrease in the total micropipe surface area.

Using photoelectron emission microscopy with hard-X-rays

We present several successful test cases of using photoelectron emission microscopy (PEEM) for photon energy up to 25 keV. First, the full extended X-ray absorption fine structure analysis was implemented in areas as small as 100 mum(2) for transition-metal K edge absorption spectra and, therefore, demonstrated the feasibility of combining structural and chemical analysis with hard-X-ray absorption spectroscopy with high lateral resolution. We also show that PEEM can be used in a transmission (radiography) mode as an imaging detector for hard-X-ray, This approach again leads to the unprecedented 0.3 mum lateral resolution, particularly critical for the use of coherence-based phase contrast techniques in real time X-ray radiology

Micropipe evolution in silicon carbide

Micropipe bundling and twisting in SiC crystals was revealed using synchrotron x-ray phase sensitive radiography. The computer simulation of micropipe evolution during the crystal growth suggests that the bundled and twisted micropipes arise under the influence of stress fields from other neighboring micropipes. The annihilation of twisted dipoles is attributed to their transformation into semiloops. Reactions of micropipe coalescence lead to the generation of micropipes and/or the annihilation of initial micropipes, resulting in the decrease in their average density.

USE OF PHOTOELECTRON MICROSCOPES AS X-RAY DETECTORS FOR IMAGING AND OTHER APPLICATIONS

We demonstrate with practical tests that a photoelectron emission microscope (PEEM) can be advantageously used as a high-lateral-resolution detector of X-rays. The advantages of this approach are discussed, in particular for coherence-based techniques

Real-time observation of Zn electro-deposition with high-resolution microradiology

We used phase contrast radiography to study the electro-deposition of Zn in real time and with high lateral resolution. Using unmonochromatic synchrotron X-rays and an optics-less imaging setup, we were able to obtain real-time radiographs of the electro-deposition in situ with gm resolution. A detailed analysis of the microstructure evolution relates the different growth parameters - such as the electric current density, the voltage bias, the pH value and the ion concentration - to very different growth morphology, ranging from film, porous, whisker and dendrite deposition. This link is both global and local. Local variations of the metal ion concentration in the electrolyte were also successfully imaged and the density profile is used to compare with the standard theory to explain the phenomenon of metal ion depletion near the electrode. The potential application of this technique to study growth with micropatterned electrodes and pulsed electric current is evaluated