About a hundred samples of y-manganese dioxide covering three materials coded SBP- A, Faradiser M and R2 have been reduced chemically by insertion of H through controlled additions of hydrazine hydrate solutions at about 1 °C. The H-inserted samples and the starting materials were subjected to chemical analysis for oxidation state, X-ray diffraction (XRD) for structure study and Fourier Transform Infrared (FTIR) spectroscopy to gain information on OH bonding. Additional techniques including FTIR spectroscopy at low temperature (~ -180 °C), electrode potential measurement and scanning electron microscopy (SEM) have also been applied. The intergrowth structure of the starting materials consisted of ramsdellite intercepted with pyrolusite layers, known as de Wolff faults, and quantified by the fraction of pyrolusite layers Pr. An additional structural parameter for these materials was the amount of micro twinning (Tw) across the 021/061 ramsdellite planes. This parameter, introduced by Pannetier, is given in percent. Values of (Pr , Tw) have been given as (0.41 , 17) for SBP-A, (0.70,10) for Faradiser M and (0.41, ~100) for R2. Upon H-insertion, the structure of the starting materials expanded homogeneously in a direction and to an extent which depended on the Pr and Tw parameters. Faradiser M, with high Pr and very low Tw, expanded homogeneously in the direction of the b lattice dimension up to an insertion level of 0.69 of s in MnOn/Hs. Above this level, the initial structure changed suddenly into the structure of the final product: the insertion then proceeded homogeneously in the new phase. The main changes were an expansion of the octahedra and a rotation leading to hinged tunnels. This is the first time that the existence of two solid solutions in the MnO2/H system has been noted. With SBP-A, the amount of microtwinning restricted the homogeneous expansion of SBP-A to s = 0.28, which occurred predominantly in the a direction. Further insertion broke the twinning boundary and formed a demicrotwinned phase of composition MnOn Ho.68 in which the tunnels were also hinged. Thereafter H-insertion proceeded heterogeneously from 0.28 to 0.68 in s. Above s = 0.68, the structure developed homogeneously towards that of the fully H-inserted product. The extensive microtwinning in R2 allowed for a homogeneous expansion, thought to be isotropic to maintain the microtwinned structure, up to s = 0.39. Higher insertion levels led to the expansion to proceed heterogeneously to a composition of MnOn Ho.63. Above s = 0.63, a new phase, the final product, was formed with fully demicrotwinned structure and fully hinged tunnels. R-insertion into y-manganese dioxide has never been reported to occur in three stages previously. The FTIR study at room temperature has shown absence of OH bond vibrations at insertion levels prior to the hinging of the tunnels, in contrast to their presence after the structure has rotated and the tunnels had hinged. This is seen as a strong indication of H mobility in the initial structure. The hinging is necessary for OH bonding as it brings the 02 and 01 oxygens closer allowing the proton to bond both covalently and by H-bonding. At low temperature, initially mobile hydrogen could be trapped and OR bonds formed only in H-inserted R2. This was linked to 061-microtwinning. The absence of OH bonds at low temperature in SBP-A and Faradiser M led to the conclusion that these materials have no 061 micro twinning faults. The absence of OH bonds at low temperature in the starting materials, particularly in R2, strongly questions the postulated OH groups in the structure of y-MnO2, according to the cation vacancy model. Electrode potential data supported the above conclusions in terms of the stages of the H-insertion. The battery activity of the materials seemed to be related to the extent at which the materials kept the initial structure with non-hinged tunnels. Comparison with previous works on the same materials suggested that the differences could be accounted for by the kinetics of the H-insertion. While protons in this work were released spontaneously on the surface of the MnO x , their diffusion into the bulk was slow due to the low temperature. In the compared literature, the reverse applies.

Pseudo-plane strain compression tests are carried out on rolled plate Zircaloy-2 using different combinations of loaded and constrained sample directions relative to the plate principal directions. Lattice strains are measured for 17 out of 18 possible measureable sample directions. The inability to obtain true plane strain led to little effect of the compression rig on deformation during elastic loading; however noticeable differences are seen when compared to similar uniaxial data for Zircaloy-2 in the plastic region. Work hardening increased with increased constraint and was affected by the configuration of loaded and constrained sample directions. Constraint showed significant effects on twinning when twinning was present. For the RD loaded cases the initiation of twinning occurs at -318 MPa for the RD/ND case (RD loaded, ND constrained direction) and -420 MPa for the RD/TD case. Intensity profiles of the (0002) and {101 ̅ 0} indicate that more twinning occurs in the RD/TD case than the RD/ND case. For TD/YD an amplification of twinning was seen in the TD/RD when compared to the TD/ND. This is indicated both by texture results as well as the intensity profiles of the (0002) and {101 ̅ 0}. Using the experimental data an elastic-plastic self-consistent (EPSC) code was used to probe the micromechanical processes that are occurring when the compression rig is operated. The experimental data was used further to constrain the hardening parameters of the EPSC code using an inverse approach. The EPSC code was able to capture the relative activity of the twinning characteristics found by the experimental data but unable to truly capture the evolution of the (0002) lattice strains when twinning occurs. / Thesis (Master, Mechanical and Materials Engineering) -- Queen's University, 2014-01-13 11:24:21.692

<p>In this study we report on the effect of the deposition parameters on the morphology and structural properties of CNTs, synthesized by means of the hot-wire chemical vapour deposition technique. SEM, Raman and XRD results show that the optimum deposition conditions for the HWCVD synthesis of aligned MWCNTs, with diameters between 50 and 150 nm and lengths in the micrometer range are: Furnace temperature of 500 &ordm / C, deposition pressure between 150 and 200 Torr, methane/hydrogen dilution of 0.67 and a substrateto- filament distance of 10 cm.</p>

This thesis contains two main parts: the first part focusses on an electron diffraction study on unsupported antimony (Sb) clusters, while in the second part the design and development of a time-of-flight mass spectrometer (TOFMS) is discussed. Electron diffraction is an ideal tool to study the structure of clusters entrained in a beam. The main advantage of this technique is the ability to study the clusters in situ and in an interaction-free environment. It is therefore not necessary to remove the particles from the vacuum system which would lead to oxidation. Since the particles do not have to be deposited on a sample for further investigation, there is also no substrate which could influence the cluster structure. An additional advantage is the short exposure to the electron beam, thereby minimising the likelihood of damaging the particles. Sb clusters were produced using an inert-gas aggregation source. To control the cluster properties the source temperature, pressure and type of cooling gas can be adjusted. In the range of source parameters tested, Sb clusters with three different structures were observed: a crystalline structure corresponding to the rhombohedral structure of bulk Sb, an amorphous structure equivalent to the structure of amorphous Sb thin films, and a structure with the same diffraction signature as Sb4 (Sb evaporates mainly as Sb4). This last structure was found to belong to large particles consisting of randomly oriented Sb4 units. In order to study the size distributions and morphologies of the Sb clusters, the clusters were deposited onto substrates and studied under an electron microscope. The crystalline particles showed a wide variety of strongly faceted shapes. Depending on source conditions, the average cluster diameters ranged from 15 to 130 nm. There was a considerable disagreement between these values and the size estimates from the diffraction results with the latter being smaller by an order of magnitude. This might be due to the existence of domains inside the clusters. The amorphous particles were all found to be spherical with mean sizes between 27 and 45 nm. The Sb4 particles showed a liquid-like morphology and tended to coalesce easily. Their sizes ranged from 18 to 35 nm. To obtain an independent method for determining the cluster size, a TOFMS was designed and developed in collaboration with Dr Bernhard Kaiser. However, the TOFMS failed to detect a cluster signal in the original set-up which is most likely due to a defective ioniser and underestimated cluster energies. Further tests were performed in a new vacuum system and mass spectra for palladium clusters were successfully recorded.

Thesis (Ph.D)--University of Adelaide, 1955. / Typewritten copy.

Thesis (M.S.)--West Virginia University, 2005. / Title from document title page. Document formatted into pages; contains x, 114 p. : ill. (some col.). Includes abstract. Includes bibliographical references (p. 112-114).

Thesis (M. Phil.)--University of Hong Kong, 1997. / Includes bibliographical references.

Thesis (M. Phil.)--University of Hong Kong, 1999. / Includes bibliographical references (leaves 107-108).

Thesis (Ph. D.)--University of Washington, 1996. / Vita. Includes bibliographical references (leaves [180]-182).

Thesis (Ph. D.)--University of Texas at Austin, 2009. / Title from PDF title page (University of Texas Digital Repository, viewed on Aug. 6, 2009). Vita. Includes bibliographical references.