Electron beam-induced crystallization of Al2O3 gate layer on ß-Ga2O3 MOS capacitors.

Electron irradiation was observed to induce crystallization of amorphous Al2O3 films grown by atomic layer deposition on ß-Ga2O3 substrates. Growth of large, strongly oriented crystalline γ-Al2O3 regions was induced using conventional-mode transmission electron microscopy (TEM) and observed to propagate outward from the interface as well as from the previously crystallized Al2O3. A few nm of epitaxial Al2O3 was already visible at the beginning of the crystallization front propagation. The phenomenon is not explained by electron beam-induced heating, which amounted to less than 1 K at all times. Direct measurement of the beam current permitted quantitative correlation between electron dose rates and crystallization rates. Enlarging the electron beam to reduce current density was found to slow the propagation of the crystallization front. Furthermore, a factor of 4 smaller electron dose was required for a given rate using 100 keV electrons as compared to 200 keV, indicating that crystallization is driven by ionization-induced atomic rearrangement within the gate layer. Lattice spacing between the oxygen sub-lattices of ß-Ga2O3 and γ-Al2O3 are favorable for the nucleation of crystallites at the interface. Multivariate statistical analysis of electron energy loss spectroscopy (EELS) data also showed evidence of diffusion between Al and Ga in the substrates and gate oxides, respectively. These structural transformations at the semiconductor-insulator interface are expected to influence the device electrical behavior and are relevant to the continued refinement of ß-Ga2O3 device technology.

Improving microstructural quantification in FIB/SEM nanotomography.

FIB/SEM nanotomography (FIB-nt) is a powerful technique for the determination and quantification of the three-dimensional microstructure in subsurface features. Often times, the microstructure of a sample is the ultimate determiner of the overall performance of a system, and a detailed understanding of its properties is crucial in advancing the materials engineering of a resulting device. While the FIB-nt technique has developed significantly in the 15 years since its introduction, advanced nanotomographic analysis is still far from routine, and a number of challenges remain in data acquisition and post-processing. In this work, we present a number of techniques to improve the quality of the acquired data, together with easy-to-implement methods to obtain "advanced" microstructural quantifications. The techniques are applied to a solid oxide fuel cell cathode of interest to the electrochemistry community, but the methodologies are easily adaptable to a wide range of material systems. Finally, results from an analyzed sample are presented as a practical example of how these techniques can be implemented.

In Situ High Temperature Synthesis of Single-Component Metallic Nanoparticles.

Nanoparticles (NPs) dispersed within a conductive host are essential for a range of applications including electrochemical energy storage, catalysis, and energetic devices. However, manufacturing high quality NPs in an efficient manner remains a challenge, especially due to agglomeration during assembly processes. Here we report a rapid thermal shock method to in situ synthesize well-dispersed NPs on a conductive fiber matrix using metal precursor salts. The temperature of the carbon nanofibers (CNFs) coated with metal salts was ramped from room temperature to ∼2000 K in 5 ms, which corresponds to a rate of 400,000 K/s. Metal salts decompose rapidly at such high temperatures and nucleate into metallic nanoparticles during the rapid cooling step (cooling rate of ∼100,000 K/s). The high temperature duration plays a critical role in the size and distribution of the nanoparticles: the faster the process is, the smaller the nanoparticles are, and the narrower the size distribution is. We also demonstrated that the peak temperature of thermal shock can reach ∼3000 K, much higher than the decomposition temperature of many salts, which ensures the possibility of synthesizing various types of nanoparticles. This universal, in situ, high temperature thermal shock method offers considerable potential for the bulk synthesis of unagglomerated nanoparticles stabilized within a matrix.

Teaching an Old Material New Tricks: Easy and Inexpensive Focused Ion Beam (FIB) Sample Protection Using Conductive Polymers.

This letter describes an innovative spin-coating system, built from off-the-shelf components, that can easily and inexpensively be integrated into any laboratory environment. Combined with a liquid suspension of conductive polymer, such a "rotary coater" enables simple coating of planar samples to create a physical protective barrier on the sample surface. This barrier aids in charge dissipation during scanning electron microscope and focused ion beam (FIB) imaging and provides wide-scale protection of the sample surface from ion bombardment during FIB imaging and gas-assisted deposition. This polymer layer replaces the localized and time-consuming electron beam deposition step typically performed during transmission electron microscopy lamella preparation. After observation, the coating can be easily removed, if desired. The described spin-coating procedure has minimal cost while providing repeatable positive results, without the need for expensive commercial coating instrumentation.

In situ observation of reversible nanomagnetic switching induced by electric fields.

We report direct observation of controlled and reversible switching of magnetic domains using static (dc) electric fields applied in situ during Lorentz microscopy. The switching is realized through electromechanical coupling in thin film Fe(0.7)Ga(0.3)/BaTiO(3) bilayer structures mechanically released from the growth substrate. The domain wall motion is observed dynamically, allowing the direct association of local magnetic ordering throughout a range of applied electric fields. During application of approximately 7-11 MV/m electric fields to the piezoelectric BaTiO(3) film, local magnetic domains rearrange in the ferromagnetic Fe(0.7)Ga(0.3) layer due to the transfer of strain from the BaTiO(3) film. A simulation based on micromagnetic modeling shows a magnetostrictive anisotropy of 25 kPa induced in the Fe(0.7)Ga(0.3) due to the strain. This electric-field-dependent uniaxial anisotropy is proposed as a possible mechanism to control the coercive field during operation of an integrated magnetoelectric memory node.

Flame synthesis of nanosized Cu-Ce-O, Ni-Ce-O, and Fe-Ce-O catalysts for the water-gas shift (WGS) reaction.

A flame synthesis method has been used to prepare nanosized, high-surface-area Cu-Ce-O, Ni-Ce-O, and Fe-Ce-O catalysts from aqueous solutions of metal acetate precursors. The particles were formed by vaporization of the precursors followed by reaction and then gas to particle conversion. The specific surface areas of the synthesized powders ranged from 127 to 163 m(2)/g. High-resolution transmission electron microscope imaging showed that the particle diameters for the ceria materials are in the range of 3-10 nm, and a thin layer of amorphous material was observed on the surface of the particles. The presence and surface enrichment of the transition-metal oxides (CuO, NiO, and Fe(2)O(3)) on the ceria particles were detected using X-ray photoelectron spectroscopy. Electron energy-loss spectroscopic studies suggest the formation of a core-shell structure in the as-prepared particles. Extended X-ray absorption fine structure studies suggest that the dopants in all M-Ce-O systems are almost isostructural with their oxide counterparts, indicating the doping materials form separate oxide phases (CuO, Fe(2)O(3), NiO) within the host matrix (CeO(2)). Etching results confirm that most of the transition-metal oxides are present on the surface of CeO(2), easily dissolved by nitric acid. The performance of the flame-synthesized catalysts was examined toward water-gas shift (WGS) activity for fuel processing applications. The WGS activity of metal ceria catalysts decreases in the order Cu-Ce-O > Ni-Ce-O > Fe-Ce-O > CeO(2) with a feed mixture having a hydrogen to carbon monoxide (H(2)/CO) ratio of 1. There was no methane formation for these catalysts under the tested conditions.