J. H. Je

Hard-x-ray microscopy with Fresnel zone plates reaches 40 nm Rayleigh resolution

Substantial improvements in the nanofabrication and characteristics of gold Fresnel zone plates yielded unprecedented resolution levels in hard-x-ray microscopy. Tests performed on a variety of specimens with 8–10keV photons demonstrated a first-order lateral resolution below 40nm based on the Rayleigh criterion. Combined with the use of a phase contrast technique, this makes it possible to view features in the 30nm range; good-quality images can be obtained at video rate, down to 50ms∕frame. The important repercussions on materials science, nanotechnology, and the life sciences are discussed.

Preferred orientation of TiN films studied by a real time synchrotron x-ray scattering

The orientational crossover phenomena in a radio frequency (rf) sputtering growth of TiN films were studied in in situ, real time synchrotron x-ray scattering experiments. For the films grown with pure Ar sputtering gas, the crossover from the (002)-oriented grains to the (111)-oriented grains occurred as the film thickness was increased. As the sputtering power was increased, the crossover thickness, at which the growth orientation changes from the 〈002〉 to the 〈111〉 direction, seemed to decrease. The addition of N2 besides Ar as sputtering gas suppressed the crossover, and consequently resulted in the (002) preferred orientation without exhibiting the crossover. We attribute the observed crossover phenomena to the competition between the surface and the strain energy. The x-ray powder diffraction, the x-ray reflectivity, and the ex situ atomic force microscopy surface topology studies consistently suggest that the microscopic growth front was in fact always the (002) planes. In the initial stage of grow...

Coherence-enhanced synchrotron radiology: Refraction versus diffraction mechanisms

Tests performed in different regimes reveal the interplay of two edge-enhancement mechanisms in radiological images taken with coherent synchrotron light. The relative weight of the two mechanisms, related to refraction and to Fresnel edge diffraction, can be changed in a controlled way. This makes it possible to obtain different images of the same object with complementary information.

Optimizing the size and surface properties of polyethylene glycol (PEG)-gold nanoparticles by intense x-ray irradiation

The polyethylene glycol (PEG) modified gold nanoparticle complex was synthesized by a one-solution synchrotron x-ray irradiation method. The impact on the structure and morphology of the gold nanoparticles of process parameters such as the PEG molecular weight, the PEG/gold molar ratio and the x-ray dosage were investigated. The size of PEG modified gold particles was found to decrease with increasing PEG addition and x-ray dosage. With the capability to monitor the absorption spectra in situ during the fast synthesis process, this opens the way to accurate control of the size and distribution. PEG chains with an intermediate length (MW6000) were found optimal for size control and colloidal stability in biologically relevant media. Our x-ray synthesized PEG-gold nanoparticles could find interesting applications in nanoparticle-enhanced x-ray tumour imaging and therapy.

Hydrogen Bubbles and the Growth Morphology of Ramified Zinc by Electrodeposition

Real-time X-ray microscopy was used to study the influence of hydrogen-bubble formation on the morphology of ramified zinc electrodeposit. The experimental results show that when intense hydrogen bubbling occurs at high potential, the morphology of the ramified zinc deposit changes from dense-branching to fern-shaped dendrite. The fern-shaped dendrite results in part from the constricted growth due to hydrogen bubbles but also from the highly concentrated electric field. The fern-shaped dendrite morphology was observed during the early stages of electroplating for both the potentiostatic and galvanostatic modes; however, the deposit plated in the galvanostatic mode densified via lateral growth during the later plating stages. This indicates that potentiostatic plating for which the hydrogen-bubble formation steadily occurs throughout the electrodeposition process is better than galvanostatic plating for fabricating fern-shaped deposits, which are ideal electrodes for Zn-air batteries due to the relatively large specific area

Effects of growth temperature on GaN nucleation layers

The effects of growth temperature on the microscopic structure of GaN nucleation layers were studied in a synchrotron x-ray scattering experiment. As the growth temperature increases from 467 to 655 °C, the stacking of GaN changes from random stacking to a mixture of cubic and hexagonal stacking. With increasing the growth temperature, the order in the atomic layer positions in the out-of-plane direction increases and the mosaic distribution becomes narrow. The optimal photoluminescence spectrum was obtained on the GaN epilayer deposited on the nucleation layer grown at 505 °C.

Thickness dependence of the crystallization of Ba-ferrite films

The crystallization of Ba-ferrite/sapphire(001) films of various thicknesses has been studied using synchrotron x-ray scattering, field emission scanning electron microscope, and atomic force microscope. In films thinner than 1000 A, Ba-ferrite amorphous precursor was crystallized into perpendicular grains keeping the magnetically easy c-axis normal to the film plane during annealing to 750 °C. In films thicker than 1000 A, however, acicular grains keeping the c-axis parallel to the film plane were grown on top of the perpendicular grains. The behavior of the saturation magnetization and the intrinsic coercivity was consistent with the thickness dependence of the crystallization. We attribute the thickness dependence of the crystallization to the substrate effect, which prefers the growth of the epitaxial, c-axis oriented perpendicular grains near the film/substrate interfacial area.

Structure determination of nanostructured Ni-Co films by anomalous x-ray scattering

Conventional x-ray diffraction failed to provide correct information on alloying of materials made of elements with close lattice parameters, even for elements commonly accepted to have miscibility. Using anomalous x-ray scattering, we showed that nanostructured NiCo films did not necessarily form solid solution as expected from their phase diagram or suggested by the results of conventional x-ray diffraction.

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