Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010.

Bis(2,2,6,6-tetramethyl-3,5-heptanedionato)zinc [Zn(TMHD)2] is a relatively uninvestigated precursor that was used in this work to grow highly c-axis-oriented ZnO films on Si(100). X-ray photoelectron spectroscopy studies before and after Ar ion sputtering indicated that surface carbon on several samples was reduced from as much as 34 at.% to much less than 1 at.% within the first 5 nm, indicating very clean Zn(TMHD)2 precursor decomposition. Microstructural and compositional analysis revealed columnar ZnO grains with domain widths of approximately half the total film thickness and a Zn-to-O atomic percent ratio indicative of stoichometric ZnO.

Thin films of 8 mol% yttria-stabilized zirconia (YSZ) of thickness ranging from 15nm-500nm have been deposited on Si3N4(90nm)/Si substrates by RF sputtering at room temperature. These samples have been studied using in situ ion scattering techniques including Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA) to analyze the oxygen distribution and defect chemistry as a function of annealing in various oxidizing and reducing ambient upto 500°C. In addition, the structural quality of these films after long time annealing has been investigated using grazing incidence X-ray diffraction (GIXRD). Temperature dependent X-ray absorption spectroscopy (XAS) has been performed to study the unoccupied density of states and chemical nature of YSZ. In this paper, we will discuss in detail the effects of annealing in different ambient on the defect chemistry, structure and stability of films in these materials systems.

A graphite wafer has been implanted with Mg+ to produce a uniform Mg concentration. Subsequent H+ implantation covered the Mg+-implanted and -unimplanted regions. Ion-beam analysis shows a higher H retention in graphite embedded with Mg than in regions without Mg. A small amount of H diffuses out of the H+-implanted graphite during thermal annealing at temperatures up to 300 °C. However, significant H release from the region implanted with Mg+ and H+ ions occurs at 150 °C; further release is also observed at 300 °C. The results suggest that there are efficient H trapping centers and fast pathways for H diffusion in the Mg+-implanted graphite, which may prove highly desirable for reversible H storage.

Oxygen uptake and conductivity were measured by nuclear-reaction analysis and alternating current impedance technique at the intermediate temperature range on sol-gel grown nanocrystalline ceria films with average grain-sizes 7 nm and 38 nm synthesized at 723 and 1173 K, respectively. Higher oxygen uptake and lower ionic conductivity were observed in ceria films with ∼7-nm grain size. High permeation-assisted oxygen diffusion in nanocrystallites combined with oxygen trapping in the disordered region contributed to higher oxygen uptake. However, the lower ionic conductivity in the film resulted from the absence of long-range lattice ordering and inactive grain-boundary/surface oxygen vacancy sites due to oxygenation. The relationship between oxygen uptake and conductivity in ceria is discussed in details by considering grain-size dependent defect density, related surface area, and enhanced oxygen mobility.

The formation of Au nanoclusters in MgO using ion implantation and subsequent annealing was investigated. Approximately 1200 and 1400 Au2+ ions/nm2 were implanted in MgO(100) substrates at 300 and 975 K, respectively. Subsequent annealing in air for 10 h at 1275 K promoted the formation of Au nanostructures in MgO. The sample implanted at 300 K showed severe radiation damage. In addition, two-dimensional plateletlike structures with possible composition of Au and MgO were formed during implantation in the sample that was implanted at 300 K. In contrast, Au implantation at 975 K promoted the nucleation of Au nanostructures during implantation. Subsequent annealing of both samples show three-dimensional clusters in MgO. However, the 975 K implanted sample shows clean, high-quality, single-crystal Au clusters that have an epitaxial relationship to MgO(100).

Multilayer films of pure ZrO2 and CeO2 were grown using molecular beam epitaxy on a yttria-stabilized zirconia (YSZ) substrate. Distinctive forbidden diffraction spots of (odd, odd, even) type were observed on the selected-area electron-diffraction patterns of the film. Dark-field imaging clearly revealed that these forbidden diffraction spots were solely due to the ZrO2 layers. Comparison of the electron diffraction pattern with that simulated by dynamical calculations suggest that the pure ZrO2 layers possess a cubic structure of space with the group P4 3m oxygen sublattice being displaced diagonally, rather than along the c axis as suggested for YSZ. Our results further suggest that the displacement of the oxygen from the ideal (¼, ¼, ¼) position might have been introduced during the film growth process.

Nucleation of gold nanoclusters in TiO2(110) single crystal using ion implantation and subsequent annealing were studied by Rutherford backscattering spectrometry /channeling (RBS/C), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Approximately 1000 Au2+/nm2 were implanted at room temperature in TiO2(110) substrates. TEM and SEM measurements reveal that rounded nanoclusters were formed during the implantation. In contrast, subsequent annealing in air for 10 hours at 1275 K promoted the formation of faceted (rectangular shaped) Au nanostructures in TiO2. RBS channeling measurements further reveled that Au atoms randomly occupied the host TiO2 lattice during the implantation. However, it appears that some Au atoms moved to the Ti lattice positions after annealing.

Oxygen (18O) diffusivity in sol-gel synthesized nano-crystalline ceria films of average grain size of 3 nm and 7 nm, annealed at 300 °C and 450 °C for one hour respectively is examined by nuclear reaction analysis (NRA). Diffusivity and electrical transport properties measured by a. c. impedance spectroscopy were compared with microcrystalline ceria film of average grain size 38 nm annealed at 900 °C for one hour. Effect of enhanced oxygen diffusion along with reduced ionic transport in nano-crystalline ceria and reduced oxygen diffusion along with enhanced ionic transport in microcrystalline ceria are correlated to long range ordering, grain boundary scattering and defect density. Enhancement in the conductivity with reduction in activation energy from 1 eV to 0.5 eV in the case 4 atom% ytterbium (Yb) doped ceria compared to pure ceria is a result of increased oxygen vacancies taking part in the defect transport.

Damage evolution and thermal recovery of 1 MeV Au2+ irradiated samarium titanate pyrochlore (Sm2Ti2O7) single crystals were studied by Rutherford backscattering spectroscopy and nuclear reaction analysis. The damage accumulation follows a nonlinear dependence on dose that is well described by a disorder accumulation model, which indicates a predominant role of defect-stimulated amorphization processes. The critical dose for amorphization at 170 and 300 K is ∼0.14 dpa, and a higher dose of ∼ 0.22 dpa is observed for irradiation at 700 K, which agrees with previous in-situ transmission electron microscopy (TEM) data for polycrystalline Sm2Ti2O7. Annealing in an 18O environment reveals a damage recovery stage at ∼ 850 K that coincides with a significant increase in 18O exchange due to oxygen vacancy mobility. This thermal recovery stage is also consistent with the critical temperature for amorphization measured by in-situ TEM in polycrystalline samples.

Gold nanoclusters dispersed in single crystal TiO2 (110) have been formed by 2MeV Au2+ implantation to an ion fluence of 1×1017 cm-2 at 300 K and 975 K followed by annealing at 1275 K for 10 hours. The morphological features, size and crystallographic orientation of the Au nanoclusters with respect to the TiO2 matrix have been investigated using conventional transmission electron microscopy and electron diffractions. In particular, the interface structure between the Au nanoclusters and TiO2 was investigated. Atomic structural model of interface between Au and TiO2 was established based on high-resolution transmission electron microscopy (HRTEM) imaging and HRTEM image simulations. Two types of orientation relationship can be identified, Au<110>//TiO2[001] and Au{111}//TiO2(200), and Au<110>//TiO2[001] and Au{111}//TiO2(110). Au clusters are faceted along Au{112}and Au{111} or Au{220} and Au{002} planes. The precipitated Au clusters show extensive (111) twins. These orientation relationships are the same for Au clusters grown on TiO2(110) surface, indicating that lowering interfacial energy to be a governing factor for setting the orientation relationship.