In this work we have investigated the intercalation of electron-donors between NbS2 slabs in Nb-based layer sulfides. Two series of Sr substituted Nb-based misfit sulfides belonging to the 1.5Q/1H and 1Q/1H series of misfit layer compounds have been synthesised. For large lanthanides (Ln=La, Ce), only the 1Q/1H compounds formed whereas for smaller lanthanides and yttrium, both types of phases can be obtained. The crystal structure of misfit sulfide (Pr0.55Sr0.45S)1.15NbS2 has been refined using the composite approach. In the Q-slab, Pr-atoms are partly replaced by Sr with a random distribution over one cation position. The crystal structure of misfit sulfide [(Sm1/3Sr2/3S)1.5]1.15NbS2 belonging to the 1.5Q/1H series have also been determined. The obtained results suggest a preferred occupancy of the cation positions in the slab where Sr atoms mainly occupy positions on the exterior of the slab while Sm atoms are in the center of the slab. The (La1-xSrxS)1.15NbS2 solid solution (0.1<x<0.9) has also been studied. It was found that the maximum value of Sr substitution is 40-50% and therefore, the minimal value of charge transfer to stabilize this structure type is about 0.6ē per Nb atom. An attempt to synthesize SrxNbS2 (0.1≤x≤0.5) intercalates was made but single phases were not obtained and increasing the temperature from 1000оС to 1100оС leads to the decomposition of these intercalates. Single crystals of Sr0.22Nb1.05S2 and Sr0.23NbS2 were found and their structures were determined. The structures belong to two different types of packings with statistical distribution of Sr between layers. A new superconducting sulfide, "EuNb2S5", was investigated by ED and HREM and its structure model consisting of Nb7S14 and (Eu3S4)2 slabs alternating along the c-axis is suggested. An attempt to suggest a model for the structure of "SrNb2S5" by means of X-ray single crystal diffraction was made. The proposed structure consists of two types of slabs: a Nb7S14 and a [Sr6(NbS4)2S] slab with niobium in tetrahedral coordination. It is shown that "SrNb2S5" and "EuNb2S5" are have similar structures. For the first time, single crystals of the complex sulfide BaNb0.9S3 have also been studied by means of X-ray single crystal diffraction. The single crystal refinement and EDX analysis showed the existence of cation vacancies at the niobium position. BaNb0.9S3 has also been studied by ED and no superstructure was found which implies that and the vacancies are statistically distributed. No improvement of the magnetic properties of the studied compounds was observed in comparison to NbS2.

Bi2Rh3Se2 have been known as a charge-density-wave (CDW) superconductor, where the superconducting critical temperature Tc and the CDW phase transition are about 0.7 K and 250 K, respectively. Since there has no definite proof that the anomaly at around 250 K comes from charge-density-wave, we wished to provide another evidence to study whether the superconductor had the properties of CDW by electric resistivity measurements applied different pressures. Bi2Rh3Se2 was prepared by using the solid state reaction method and heating in the quartz tube. After the sample was synthesized, the quality was identified by XRD, MPMS, and specific heat probe. With the confirmation of the above-mentioned measurements, we can determine the sample¡¦s quality is good. Furthermore, temperature-dependent resistivity (2-340 K) under pressure (up to 22.23 kbar) on the ternary superconductor Bi2Rh3Se2 are performed to study the possible coexistence of CDW and superconductivity. Interestingly, the resistive anomaly occurred at Ts~250 K, is shifted to higher temperature with increasing pressure. This experimental finding is not consistent with a traditional CDW transition. Moreover, the temperature-dependent Transmission Electron Microscopy (TEM) electron diffraction is evident a structural phase transition from space group ¡§C1 2/m 1¡¨ (Ts > 250 K) to ¡§P1 2/m 1¡¨ (Ts < 250 K). Finally, We do the Co doping to make sure the effects of chemical pressure on this phase transition. The results are opposite to imposed by physical pressure that the transition is shift to lower temperature with more Co inside the sample.

Thesis (Ph. D.)--University of Missouri-Columbia, 2000. / Typescript. Vita. Includes bibliographical references (leaves 139-143). Also available on the Internet.

Thesis (Ph. D.)--University of Missouri-Columbia, 2000. / Typescript. Vita. Includes bibliographical references (leaves 139-143). Also available on the Internet.

published_or_final_version / Physics / Master / Master of Philosophy

The Tin dioxide (SnO2) and Titanium dioxide (TiO2) are very promising materials in Material science. The SnO2 is commonly used as a gas sensor while the TiO2 is used as a catalyst in many reactions. Despite of the usefulness of these two substances, their surface structures lack detail investigations in the previous years. The Low Energy Electron Diffraction (LEED) technique is commonly used to characterize surfaces in the past 40 years, it is a mature system that many researches rely on its result. However, structural analysis in LEED requires comparison with computational results based on pre-defined structure models, which is a time-consuming method and the results are not guaranteed to be found. The direct determinations of structure by Patterson function inversion methods introduced by Huasheng Wu and S. Y. Tong could provide a different path to search for surface structure. In the Patterson function, each maximum in the function corresponds to a relative position vector of atomic pairs. Multiple-angle-incident LEED has to be performed to obtain an artifact-free Patterson function. Serveal SnO2 and TiO2 surfaces have been characterized by LEED and Patterson function inversion. SnO2 (110), (100), (101) , Rutile TiO2 (110), Anatase TiO2 (110) have been prepared by argon ion sputtering and annealing cycles and the cleanness has been checked by Auger Electron Spectroscopy and LEED. Reconstruction is observed based on the study of the LEED patterns. SnO2 (110) surface shows a 4 x 1 reconstruction in UHV environment while it gives 1 x 1 under annealing in oxygen and C(2 x 2) at higher annealing temperature afterward. SnO2 (100) , (101) and Rutile TiO2 (110) surfaces show 1 x 1 reconstruction in UHV environment and the reconstruction persists for further annealing. The Anatase TiO2 (110) surface shows a 3 x 4 reconstruction in UHV environment. The 3 x 4 reconstruction of Anatase TiO2 (110) surface would raise research interests as it is quite a special reconstruction. Multiple-angle-incident LEED has been performed on the SnO2 (100), (101) and Rutile TiO2 (110) surfaces. Patterson function inversion is performed on the surfaces SnO2 (100) and Rutile TiO2 (110) . Only LEED is performed on SnO2 (110) , (101) and Anatase TiO2 (110) surfaces. From Patterson functions analysis, the surface atoms positions are determined for the surface SnO2 (100) and Rutile TiO2 (110). The results show that their reconstructions are negligible, but they have obvious relaxations. / published_or_final_version / Physics / Master / Master of Philosophy

abstract / Physics / Doctoral / Doctor of Philosophy

The main objective of this work is the fundamental physical study of individual isolated carbon nanostructures in order to address their intrinsic vibrational and optical properties and also to estimate and quantify the environmental effects. For these purposes, we synthesized individual single- and multi-walled carbon nanotubes by chemical vapour deposition method on dedicated substrates. The main aspect of the work involves the combined use of different experimental probes on the same individual nanostructures. We performed a complete structure analysis by electron diffraction and high-resolution electron microscopy and the measurement of the Raman spectra on these individual nanostructures. Several important environmental effects were evidenced for the first time, e.g. the effect of mechanical coupling (van-der-Waals interaction) between the layers of double-walled carbon nanotubes leading to the change in the low-frequency Raman modes and the optical resonance conditions. Moreover the behaviour of high-frequency modes of double-walled tubes was also analysed and described. As a result of this work several experimental criteria for structure diagnostics of multi-walled carbon nanotubes were proposed.

Ultrafast electron diffraction is a novel pump-probe technique which aims to determine transient structures during photoinduced chemical reactions and other structural transitions. This technique provides structural information at the atomic level of inspection by using an electron pulse as a diffractive probe. The atomic motions of interest happen on the 100 fs = 10^(−13) s time scale. To observe these atomic motions, a probe which matches this time scale is required. In this thesis, I describe the development of an electron diffractometer which is capable of 200 fs temporal resolution while maintaining high signal level per electron pulse. This was made possible by the construction of an ultra-compact photoactivated 60 keV femtosecond electron gun. Traditional electron pulse characterization methods are unsuitable for high number density femtosecond electron pulses such as the pulses produced by this electron gun. I developed two techniques based on the laser ponderomotive force to reliably determine the duration of femtosecond electron pulses into the sub-100 fs range. These techniques produce a direct cross-correlation trace between the electron pulse and a laser pulse. The results of these measurements confirmed the temporal resolution of the newly developed femtosecond electron diffractometer. This cross-correlation technique was also used to calibrate a method for the determination of the temporal overlap of electron and laser pulses. These techniques provide the pulse diagnostics necessary to utilize the temporal resolution provided by femtosecond electron pulses. Owing to their high charge-to-mass ratio, electrons are a sensitive probe for electric fields. I used femtosecond electron pulses in an electron deflectometry experiment to directly observe the transient charge distributions produced during femtosecond laser ablation of a silicon (100) surface. We found an electric field strength of 3.5 × 10^6 V/m produced by the emission of 5.3 × 10^11 electrons/cm^2 just 3 ps after an excitation pulse of 5.6 J/cm^2 . This observation allowed us to rule out Coulomb explosion as the mechanism for ablation under the conditions present in this experiment.

Thesis (Ph. D.)--University of Washington, 1997. / Vita. Includes bibliographical references (leaves [161]-163).