Analysis of the shapes of diffraction peak profiles (DPPA) is a widely used method for characterising the microstructure of crystalline materials. The DPPA method can be used to determine details about a sample that include, the micro-strain, crystal size or dislocation cell size, dislocation density and arrangement, quantity of planar faults and dislocation slip system population.The main aim of this thesis is to evaluate the use of DPPA in studying the deformation of metals. The alloys studied are uni-axially deformed samples of nickel alloy, nickel-200, 304 and 316 stainless steel alloys and titanium alloys, Ti-6Al-4V and grade 2 CP-titanium.A number of DPPA methods were applied to these metals: a full-width method; a method that attributes size and strain broadening to the Lorentzian and Gaussian integral breadth of a Voigt; different forms of the variance method; the Williamson-Hall method; the alternative method; and variations of the Warren-Averbach method. It is found that in general the parameters calculated using the different methods qualitatively agree with the expectations and differences in the deformation of the different metals. For example, the dislocation density values found for all metals, are approximately the same as would be expected from TEM results on similar alloys. However, the meaning of the results are ambiguous, which makes it difficult to use them to characterise a metal. The most useful value that can be used to describe the state of a metal is the full-width. For a more detailed analysis the Warren-Averbach method in a particular form, the log format fitted to individual Fourier coefficients, is the most useful method.It was found that the shape of different diffraction peaks change in different texture components. These changes were found to be different for the different metals. A method to calculate the shape of diffraction peaks, in different texture components, using a polycrystal plasticity models was investigated. It was found that for FCC metals, the use of a Taylor model was able to qualitatively predict the changes in the shape of diffraction peaks, measured in different texture components. Whereas, for titanium alloys, a model which used the Schmid factor was able to qualitatively explain the changes. The differences in the FCC alloys was attributed to being due to differences in the stacking fault energy of the alloys. For nickel, which develops a heterogeneous cell structure, an additional term describing changes in the crystal size in different orientations is required. The differences between the titanium alloys were shown to be due the presence of twinning in CP-titanium and not in Ti-6Al-4V. This difference was thought to cause an additional broadening due to variations in intergranular strains in twinned and non-twinned regions. The use of polycrystal plasticity models, to explain the shape of diffraction peaks, raises questions as to the validity of some of the fundamental assumptions made in the use of most DPPA methods.

Automated narrow-gap girth-butt welds are replacing conventional welding methods to join sections of austenitic stainless steel pipe in the primary circuit of Pressurised Water Reactors, to reduce manufacturing costs and improve quality. To ensure the safe operation of these systems, reliable structural integrity assessments have to be undertaken, requiring the mechanical properties of welded joints to be characterised alongside the weld residual stress magnitude and distribution.This research project characterised, for the first time, the weld residual stress field and the tensile and ductile fracture toughness properties of a 33 mm thick narrow-gap 304L stainless steel pipe weld. The residual stress was characterised using two complementary approaches: deep hole drilling and neutron diffraction. A novel neutron diffraction scanning technique was developed to characterise the residual stress field, without cutting an access window into the component, leaving the original weld residual stress field undisturbed. A modified deep hole drilling technique was developed to characterise the residual stress retained in fracture mechanics specimens extracted from the pipe weld in two orientations. The modified technique was shown to measure the original weld residual stress field more accurately than through conventional deep hole drilling. Residual stresses, exceeding 50% of the weld material proof strength, were retained in axially-orientated fracture mechanics specimens.Tensile tests showed that the weld was approximately 60% overmatched. It was demonstrated that neither retained residual stress, nor specimen orientation, had a discernible effect on the measured fracture toughness of the weld material. In less ductile materials, however, the level of retained residual stress may unduly influence the measurement of fracture toughness. At initiation, the fracture toughness properties of both the parent and weld materials were far in excess of the measuring capacity of the largest fracture mechanics specimens that could be machined from the weld.The influence of residual stress and fracture toughness on the performance of narrow-gap welded pipework was investigated. Full elastic-plastic finite element analyses were used to model the pipe weld, containing a postulated defect under combined primary and secondary loading. The results, applied within the framework of an R6 structural integrity assessment, compared different plasticity interaction parameters on the prediction of failure load; the conventional ρ-parameter approach was compared with the recently developed, more advanced, g-parameter. It was shown that the g-parameter significantly reduced the conservatism of the ρ-parameter approach. However, for this pipe weld, plastic collapse was predicted to precede failure by ductile initiation, suggesting that a plastic collapse solution may be an appropriate failure criterion to use in structural integrity assessments of similar component and defect combinations.

Title: The magnetocrystalline anizotropy in the TbTX compounds Author: Milan Klicpera Department: Department of Condensed Matter Physics Supervisor: doc. Mgr. Pavel Javorský, Dr. Supervisor's e-mail address: javor@mag.mff.cuni.cz Abstract: The subject of this work is the study of structural, magnetic and trans- port properties of the TbNi(Al,In) series to finding connections between magne- tocrystalline anisotropy and lattice parameters of the structure of the TbTX com- pounds. Polycrystalline TbNiAl1−xInx samples were prepared by melting. The phase and crystal structure analysis were provided on samples. We performed the measurements of the magnetization, susceptibility, specific heat, resistivity, low temperature X-ray diffraction and powder neutron diffraction. From the neutron diffraction data we refined lattice parameters and propagation vectors of the series. The main propagation is (000) and second weaker component has the propagation vector (1 2 0 1 2 ). The change of the magnetocrystalline anisotropy from uniaxial to planar type occurs for compounds with x between 0.4 and 0.5. Keywords: magnetization, X-ray and neutron diffraction, electrical resistivity.

The deformation mechanisms of commercially pure magnesium using advanced in-situ methods were investigated in the present work. Compression and tensile test were done at room temperature. Simultaneously, the neutron diffraction was measured and the acoustic emission was recorded. The microstructure of the deformed material was also studied by means of optical microscopy and electron back-scattered diffraction. These measurements provided information about twin nucleation and growth, microstructure changes and the influence of the orientation of grains on the number of twins and their shape. The values obtained were compared to the Elasto-Plastic Self-Consistent model, which provides information about the activity of deformation mechanisms. We focused on clarifying the influence of twinning activity on asymmetry between tensile and compression deformation.

The work is focused on developing testing methods for investigating of the deformation mechanisms of magnesium alloys. The work involves the measurement of in-situ acoustic emission and neutron diffraction and comparison to the theoretical models. Mg + 1wt.% Zr alloy was selected for investigation of the compression - tension asymmetry. Advanced analysis of acoustic emission and neutron diffraction data revealed activation of different slip systems during deformation. Moreover, the different evolution of twinning was explained. The same methods were used to investigate the aluminum influence on deformation mechanisms. The hardening of basal slip and twinning and increasing importance of prismatic slip was observed.

The hydrogenation of Zintl phases enables the formation of new structural entities with main group elementhydrogen bonds in the solid state. The hydrogenation of SrSi, BaSi and BaGe yields the hydrides SrSiH5/3-x, BaSiH5/3-x and BaGeH5/3-x. The crystal structures show a six-fold superstructure compared to the parent Zintl phase and were solved by a combination of X-ray, neutron and electron diffraction and the aid of DFT calculations. Layers of connected HSr4 (HBa4) tetrahedra containing hydride ions alternate with layers of infinite single- and double-chain polyanions, where hydrogen atoms are covalently bound to silicon and germanium. The idealized formulae AeTtH5/3 (Ae = alkaline earth, Tt = tetrel) can be rationalized with the Zintl-Klemm concept according to (Ae2+)3(TtH-)(Tt2H2-)(H-)3, where all Tt atoms are three-binding. The non-stoichiometry (SrSiH5/3-x, x = 0.17(2); BaGeH5/3-x, x = 0.10(3)) can be explained by additional π-bonding of the Tt chains.

Hydrogenation products of the Zintl phases AeTt (Ae = alkaline earth; Tt = tetrel) exhibit hydride anions on interstitial sites as well as hydrogen covalently bound to Tt which leads to a reversible hydrogenation at mild conditions. In situ thermal analysis, synchrotron and neutron powder diffraction under hydrogen (deuterium for neutrons) pressure was applied to BaTt (Tt=Ge, Sn). BaTtHy (1<y<1.67, γ-phases) were formed at 5 MPa hydrogen pressure and elevated temperatures (400–450 K). Further heating (500–550 K) leads to a hydrogen release forming the new phases β-BaGeH0.5 (Pnma, a=1319.5(2) pm, b=421.46(2) pm, c=991.54(7) pm) and α-BaSnH0.19 (Cmcm, a=522.72(6) pm, b=1293.6(2) pm, c=463.97(6) pm). Upon cooling the hydrogen rich phases are reformed. Thermal decomposition of γ-BaGeHy under vacuum leads to β-BaGeH0.5 and α-BaGeH0.13 [Cmcm, a=503.09(3) pm, b=1221.5(2) pm, c=427.38(4) pm]. At 500 K the reversible reaction α-BaGeH0.23 (vacuum)⇄β-BaGeH0.5 (0.2 MPa deuterium pressure) is fast and was observed with 10 s time resolution by in situ neutron diffraction. The phases α-BaTtHy show a pronounced phase width (at least 0.09<y<0.36). β-BaGeH0.5 and the γ-phases appear to be line phases. The hydrogen poor (α- and β-) phases show a partial occupation of Ba4 tetrahedra by hydride anions leading to a partial oxidation of polyanions and shortening of Tt–Tt bonds.

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Intercritically austempered ductile iron (IADI) with a matrix microstructure of ferrite plus metastable austenite has an excellent combination of strength and toughness. The high strength and good ductility of this material is due to the transformation of metastable austenite to martensite during deformation. In the present study, the transformation of austenite to martensite for intercritically austempered ductile irons of varying alloy chemistry (varying amounts of nickel and/or manganese) were examined using in-situ neutron diffraction under strain-controlled loading at VULCAN at the Spallation Neutron Source at Oak Ridge National Laboratory (ORNL). Both diffraction and tensile data were collected and synced using the VDRIVE software (a proprietary ORNL software package). The single peak fit method was employed in the analysis of the diffraction data. In this thesis, the stress and strain for the start of the transformation of metastable austenite to martensite were determined. The development of residual stresses during deformation and the elastic diffraction constants for both the ferrite and austenite phases were also determined. The material was characterized using optical microscopy, backscattered imaging in the scanning electron microscopy, energy dispersive spectroscopy and transmission electron microscopy. / Master of Science

No description available.