Ultrasonic Study Of The Elastic Properties And Phase Transitions In Selected Mixed Sulphate Crystals

The thesis investigated the elastic properties and phase transitions in selected mixed sulphate crystals – Lithium Hydrazinium Sulphate [LiN2H2SO4], Lithium Ammonium Sulphate [LiNH4SO4] and Lithium Potassium Sulphate [LiKSO4] – using ultrasonic technique. The pulse echo overlap technique has been used for measuring ultrasonic velocity and its dependence on temperature along different directions with waves of longitudinal and transverse polarizations. Two major numerical techniques and the corresponding computer programs developed as part of present work are presented in this thesis. All the 9 elastic constants of LHS are determined accurately from ultrasonic measurements and applying misorientation correction refines the constants. Ultrasonic measurements are performed in LAS to determine the elastic constants and to study the low temperature phase transitions. Temperature variation studies of elastic constant of LAS are performed for 6 different modes of propagation for heating and cooling at low temperatures. All the 5 independent elastic constants of LPS is determined using ultrasonic measurements. It is concluded that LPS crystal does not undergo a phase transition near this temperature. A comparison of the three crystals studied shows that LPS has maximum number of phase transitions and LHS has the least number. It is interesting to note that LPS has the simplest formula unit among the three. There is considerable scope for the future work on these crystals and others belonging to the sulphate family.

Influence of quantum-dots density on average in-plane strain of optoelectronic devices investigated by high-resolution X-ray diffraction

High-resolution X-ray diffractometry is used to probe the nature of a diffraction-peak broadening previously noticed in quantum dots (QDs) systems with freestanding InAs islands on top of GaAs (001) substrates [Freitas et al., Phys. Status Solidi (A) 204, 2548 (2007)]. The procedure is hence extended to further investigate the capping process of InAs/GaAs QDs. A direct correlation is established between QDs growth rates and misorientation of lattice-planes at the samples surfaces. This effect provides an alternative too] for studying average strain fields on QDs systems in standard triple axis diffractometers running on X-ray tube sources, which are much more common than synchrotron facilities. (C) 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Fragmentation of orientation within grains of a cold-rolled interstitial-free steel

The formation of a favourable recrystallization texture in interstitial-free (IF) steels depends on the availability and activation of particular nucleation sites in the deformed microstructure. This paper presents a description of the deformed microstructure of a commercially cold-rolled IF steel, with particular emphasis on the microstructural inhomogeneities and short-range orientational variation that provide suitable nucleation sites during recrystallization. RD-fibre regions deform relatively homogeneously and exhibit little short-range orientational variation. ND-fibre regions are heavily banded and exhibit considerable short-range orientational variation associated with the bands. While the overall orientational spread of ND-fibre grains frequently is about the ND-axis, the short-range orientational variation often involves rotation about axes in the TD-ND plane that are nearer to the TD than the ND.

Generating misorientations in shear deformation structures

Of considerable importance to the generation of ultrafine microstructures is the development of high misorientations. The present work examines the effect of the crystallographic rotation field in simple shear upon the evolution of misorientation during plastic working. A series of Taylor simulations are presented and it is shown that the rotation field is such that small differences in orientation in the region of the main torsion texture components are considerably increased with the application of shear strain. This did not occur in simulations of rolling. The torsion simulations compare favourably with the nature of the misorientations evident in hot worked 1050 Al and Ti-IF steel. It is concluded that shear deformation, by its nature, facilitates the generation of higher misorientations.

Understanding the deformed microstructure of cold-rolled IF and LC steel

This paper presents an overview of a series of investigations of the microstructure and texture of cold-rolled IF and LC steel. The investigations made extensive use of orientation mapping using electron backscattered diffraction (EBSD) in a field emission gun scanning electron microscope (FEG-SEM). The effect of grain boundaries on the deformed microstructure was examined by comparing the textures of regions near grain boundaries and in the interiors of grains.  A general weakening of the texture, but a strengthening of the {OOI}<110> component, occurs in the vicinity of grain boundaries. Misorientation angle and axis distributions were used to characterise the fragmentation of grains belonging to different orientation classes. The influence of carbon on the deformed microstructure and nucleation during recrystallization was clarified by examining the microstructures of LC and IF steels during rolling and annealing. The
results of the investigations emphasize the important role of shear banding in determining the fragmentation behaviour of ND-fibre grains and the orientations of viable recrystallization nuclei within the deformed microstructure.

The effect of multiple deformations on the formation of ultrafine grained steels

A C-Mn-Nb-Ti steel was deformed by hot torsion to study ultrafine ferrite formation through dynamic strain-induced transformation (DSIT) in conjunction with air cooling. A systematic study was carried out first to evaluate the effect of deformation temperature and prior austenite grain size on the critical strain for ultrafine ferrite formation (ε C,UFF) through single-pass deformation. Then, multiple deformations in the nonrecrystallization region were used to study the effect of thermomechanical parameters (i.e., strain, deformation temperature, etc.) on ε C,UFF. The multiple deformations in the nonrecrystallization region significantly reduced ε C,UFF, although the total equivalent strain for a given thermomechanical condition was higher than that required in single-pass deformation. The current study on a Ni-30Fe austenitic model alloy revealed that laminar microband structures were the key intragranular defects in the austenite for nucleation of ferrite during the hot torsion test. The microbands were refined and overall misorientation angle distribution increased with a decrease in the deformation temperature for a given thermomechanical processing condition. For nonisothermal multipass deformation, there was some contribution to the formation of high-angle microband boundaries from strains at higher temperature, although the strains were not completely additive.

Dynamic softening of ferrite during large strain warm deformation of a plain-carbon steel

The evolution of dynamic ferrite softening in a plain-carbon steel was investigated by torsion tests during warm deformation at 810 °C, in the two-phase (ferrite + austenite) region, and strain rate of 0.1 s−1 with different strains up to 50. The warm flow behaviour and ferrite microstructural parameters, such as grain size, misorientation angle across ferrite/ferrite boundaries, and the fraction of high-angle and low-angle grain/subgrain boundaries were quantified using electron back scatter diffraction. The results show that with increasing strain up to not, vert, similar2, the ferrite grain size and fraction of high-angle boundaries rapidly decrease and the fraction of low-angle boundaries increases. However, these parameters remain approximately unchanged with increasing strain from not, vert, similar2 to 50. The dynamic softening mechanism observed during large strain ferritic deformation is explained by dynamic recovery and continuous dynamic recrystallization.

Modeling the flow behavior, recrystallization, and crystallographic texture in hot-deformed Fe-30 Wt Pct Ni Austenite

The present work describes a hybrid modeling approach developed for predicting the flow behavior, recrystallization characteristics, and crystallographic texture evolution in a Fe-30 wt pct Ni austenitic model alloy subjected to hot plane strain compression. A series of compression tests were performed at temperatures between 850 °C and 1050 °C and strain rates between 0.1 and 10 s⁻¹. The evolution of grain structure, crystallographic texture, and dislocation substructure was characterized in detail for a deformation temperature of 950 °C and strain rates of 0.1 and 10 s⁻¹, using electron backscatter diffraction and transmission electron microscopy. The hybrid modeling method utilizes a combination of empirical, physically-based, and neuro-fuzzy models. The flow stress is described as a function of the applied variables of strain rate and temperature using an empirical model. The recrystallization behavior is predicted from the measured microstructural state variables of internal dislocation density, subgrain size, and misorientation between subgrains using a physically-based model. The texture evolution is modeled using artificial neural networks.

Evaluation of selective growth in a Fe-2.8% Si single crystal using Rodrigues-Frank space

A Fe-2.8%Si single crystal was scratched in order to randomise the texture in the neighbourhood of the notch. Annealing resulted in recrystallization and grain growth starting from the deformed zone. Misorientations between the single crystal matrix and the grown grains were gathered and were studied in order to investigate the possibility for selective growth based on a specific misorientation. However, instead of studying the misorientation angle or axis profiles separately in a 1D or 2D projection a full misorientation analysis was carried out in the 3-dimensional Rodrigues-Frank misorientation space, which offers an unambiguous interpretation of the data because no features are hidden or masked by a projection. It is concluded that the selective growth phenomenon following the <110>26.5deg misorientation relationship is strongly supported by the gathered orientation data, after appropriately normalizing these data with respect to a random misorientation distribution.

Characterization on ferrite microstructure evolution during large strain warm torsion testing of plain low carbon steel

Ferrite grain/subgrain structures evolution during the extended dynamic softening of a plain low carbon steel was investigated throughout the large strain warm deformation by hot torsion. Microstructural analysis with electron back-scattering diffraction (EBSD) scanning electron microscope (FEG/SEM) was carried out on the ferrite microstructural parameters. The results showed that the warm flow stress–strain curves are similar to those affected only by dynamic softening and an extended warm flow softening is seen during large strain deformation up to 30. Furthermore, with an increase in strain up to ~ vert, similar1 the grain size of ferrite, misorientation angle and fraction of high-angle boundaries gradually decrease and fraction of low-angle boundaries increases. With a further increase in the strain beyond ~, vert, similar2, these parameters remain approximately unchanged. No evidence of discontinuous dynamic recrystallisation involving nucleation and growth of new grains was found within ferrite. Therefore, the dynamic softening mechanism observed during large strain ferritic deformation is explained by continuous dynamic recrystallization (CDRX).

Non-Schmid behaviour during secondary twinning in a polycrystalline magnesium alloy

The present work combines electron backscattering diffraction and Schmid analysis to investigate secondary twinning in the magnesium alloy Mg–3Al–1Zn. Inspection of the misorientations between the parent and ^{{1011} - {1012}} doubly twinned volumes reveals that there are four possible variants. One of these variants (the one that forms a misorientation with the matrix characterized by 38°^⟨1210⟩ ) is favoured much more than the others. This variant involves the activation of secondary twinning systems quite inconsistent with Schmid-type behaviour. For the secondary twin to grow significantly it must take on a shape enforced by the primary twin. This is non-optimal for strain compatibility. It is argued that the 38°^⟨1210⟩ variant occurs most because it provides the closest match between the primary and secondary twinning planes, thus minimizing the compatibility strain.

Characteristics of the contraction twins formed close to the fracture surface in Mg-3A1-1Zn alloy deformed in tension

Characteristics of the “contraction” twins, formed close to the fracture surface in Mg–3Al–1Zn alloy deformed in tension approximately perpendicular to the grain c-axes, are investigated using transmission electron microscopy. The grain c-axis contractions were largely accommodated by {1011}-{1012} source double-twins in a variant characterized by 38° ⟨1210⟩ source twin/matrix misorientation in conjunction with dislocation slip. A possible interpretation of the observed preference for this variant formation is given and some crystal plasticity modelling is performed to elucidate the matter.

Identification and rationalization of secondary twin variants in a magnesium alloy

The present work combines electron backscatter diffraction, transmission electron microscopy and Schmid analysis to investigate secondary twinning in the magnesium alloy Mg-3AI-1Zn. Inspection of the misorientations between the parent matrix and {1011} - {1012} doubly twinned volumes reveals that there are four possible variants. One of these variants characterized by 38°< 1210 > misorientation with the matrix is favoured much more than the others. This variant involves activation of the secondary twinning systems that are quite inconsistent with the Schmid-type behaviour. For the secondary twin to grow significantly it must take on a shape enforced by the primary twin, however, this is not optimal for strain compatibility. It is argued that the 38° < 1210 > variant occurs most frequently because it provides the closest match between the primary and secondaty twinning planes, thus minimizing the compatibility strain. This conjecture is confirmed by the simulations of twin activity m ellipsoidal grains performed using the visco-plastic self-consistent crystal plasticity model.

Electron back scattered diffraction (EBSD) characterization of warm rolled and accumulative roll bonding (ARB) processed ferrite

An interstitial free (IF) steel was severely deformed using accumulative roll bonding (ARB) process and warm rolling. The maximum equivalent strains for ARB and warm rolling were 4.8 and 4.0, respectively. The microstructure and micro-texture were studied using optical microscopy and scanning electron microscopy equipped with electron back scattered diffraction (EBSD). The grain size and misorientation obtained by both methods are in the same range. The microstructure in the ARB samples after 6 cycles is homogeneous, although a grain size gradient is observed at the layers close to the surface. The through thickness texture gradient in the ARB samples is different from the warm rolled samples. While a shear texture (⟨110⟩//rolling plane normal direction (ND)) at the surface and rolling texture at the center region is developed in the ARB  samples, the overall texture is weak. The warm rolled samples display a sharp rolling texture through the thickness with increasing the sharpness toward the center. These differences are attributed to the fact that the central region of ARB strip is comprised of material that was once at the surface. The ARB process  can suppress the formation of shear bands which are conventional at warm rolled IF steels. EBSD study on the sample with 6th cycle of ARB following the annealing at 750 ◦C verified a texture gradient through the thickness of the sheet. The shear orientations at the surface and at the quarter thickness layers can be identified even after annealing. The overall weak texture and existence of shear orientations make ARB processed samples unfavorable for sheet metal forming in compare with warm rolled samples.