Defect characterization of KTP single crystals

Potassium titanyl phosphate (KTP) is a relatively new nonlinear optical material with excellent combination of physical properties. This paper presents the combined etching and X-ray topographic studies carried out on KTP crystals with a view to characterizing their defects. KTP crystals employed in this investigation were grown from flux. Optical microscopic study of habit faces revealed growth layers and growth hillocks on (100) and (011) faces respectively. Etching of (011) habit faces proved that growth hillocks corresponded to the emergence point of dislocation out crops on these faces. The suitability of the new etchant to reveal dislocation was confirmed by etching the matched pairs obtained by cleaving. The defects present in the crystal were also studied by X-ray topography. The defect configuration in these crystals is characteristic of crystals grown from solution. The dislocations arc predominantly linear with their origin either at the nucleation centre or inclusions. In general, grown crystals were found to have low dislocation density and often large volumes of crystals free from dislocation could be obtained.

Dislocation characterization in crystals of potash alum grown by seeded solution growth under conditions of low supersaturation

An analysis has been carried out of the genesis and character of growth dislocations present in all growth sectors of single crystals of potash alum. The crystals, grown from seeded solutions by the temperature lowering method under conditions of low supersaturation, presented the well-developed forms: {111} dominant, {100} and {110}. Growth dislocations formed predominately during refacetting of the edges and corners of the seed, rounded during preparation and insertion into the supersaturated solution. From here they become refracted into the {111} sectors which proved to be the most defective. Smaller numbers of dislocations form at the {111}, {100} and {110} seed interfaces and propagate in these sectors. In crystals of inferior quality, a number of inclusions were found predominantly in the fast growing {100} sectors which become the source of additional dislocations. Dislocations present in the original seed did not propagate across the interface into the developing crystal. Dislocations of all characters were observed. The principal Burgers vectors were found to be left angle bracket100right-pointing angle bracket, left angle bracket110right-pointing angle bracket and left angle bracket111right-pointing angle bracket.

Kinetic approach to dislocation bending in low-mobility films

A kinetic model has been developed for dislocation bending at the growth surface in compressively stressed low-mobility films such as III-V nitrides. It is based on a reduction in the number of atoms at the growth surface. Stress and nonstress sources of driving force for such a reduction are discussed. A comparison between the derived equations and experimentally measured stress evolution data yields good agreement between the predicted and observed angles through which dislocations bend.

Growth and extraction of flux free YBCO crystals

An improved flux draining technique for the extraction of grown YBCO crystals from its solvent is reported. This simple and efficient technique facilitates in-situ flux separation in the isothermal region of the furnace. Consequently, the crystals are spared from thermal shock and subsequent damage. Flux-free surfaces of these crystals were studied by optical microscopy. Transmission X-ray topographs of the crystals reveal the dislocations present in them as well as the stresses developed as a result of ferroelastic phase transition occurring during cooling.

Dynamic recrystallisation during hot working of Zr-2 center dot 5Nb: Characterisation using processing maps

The characteristics of the hot deformation of Zr-2.5Nb (wt-%) in the temperature range 650-950 degrees C and in the strain rate range 0.001-100 s(-1) have been studied using hot compression testing. Two different preform microstructures: equiaxed (alpha + beta) and beta transformed have been investigated. For this study, the approach of processing maps has been adopted and their interpretation carried out using the dynamic materials model. The efficiency of power dissipation given by [2m/(m + 1)], where m is the strain rate sensitivity, is plotted as a function of temperature and strain rate to obtain a processing map. A domain of dynamic recrystallisation has been identified in the maps of equiaxed (alpha + beta) and beta transformed preforms. In the case of equiaxed (alpha + beta), the stress-strain curves are steady state and the dynamic recrystallisation domain in the map occurs with a peak efficiency of 45% at 850 degrees C and 0.001 s(-1). On the other hand the beta transformed preform exhibits stress-strain curves with continuous flow softening. The corresponding processing map shows a domain of dynamic recrystallisation occurring by the shearing of alpha platelets followed by globularisation with a peak efficiency of 54% at 750 degrees C and 0.001 s(-1). The characteristics of dynamic recrystallisation are analysed on the basis of a simple model which considers the rates of nucleation and growth of recrystallised gains. Calculations show that these two rates are nearly equal and that the nucleation of dynamic recrystallisation is essentially controlled by mechanical recovery involving the cross-slip of screw dislocations. Analysis of flow instabilities using a continuum criterion revealed that Zi-2.5Nb exhibits flow localisation at temperatures lower than 700 degrees C and strain rates higher than 1 s(-1).

Sintering of beta titanium: Role of dislocation pipe diffusion

Sintering of titanium in its high temperature beta phase was studied by isothermal dilatometry. The sintering shrinkage y did not follow the normal time exponent type of behaviour, instead being described by the equation y = Kt(m)/[1-(A+Bt)(2)], where m = 1.93 +/- 0.07, with an activation energy of 62-90 kJ mol(-1). A detailed analysis of these results, based on the 'anomalous' diffusion behaviour reported for beta titanium, is carried out. It is shown that the generation of a high density of dislocations during the alpha --> beta phase transformation, coupled with sluggish recovery at the sintering necks, enables sintering mass transport by pipe diffusion through dislocation cores from sources of matter within the particles to become dominant.

Electron microscopy and diffraction of ordering in Ni---W alloys

Electron microscopy and diffraction studies of ordering in stoichiometric Ni-20%W and off-stoichiometric Ni-15%W alloys have been carried out. The specimens of Ni-20%W were first disordered at 1398 K for 4 h and then quenched rapidly into water. Short range order (SRO) spots were observed at {1 1/2 0}* positions. Two hitherto unknown metastable phases: D-2h(25)-Ni2W and DO22-Ni3W were observed in the diffraction patterns. Long range order (LRO) transformations were studied at 1103 and 1213 K. Kinetics and mechanism of transformations have been identified. Ni-15%W specimens were solution treated at 1523 K for 1 h followed by quenching in water. SRO spots similar to those found in Ni-20%W were observed in this alloy as well. The transition to LRO was studied at 1093 K. Distinct Ni4W precipitates could be observed after 5 h of annealing at this temperature. After 100 h of annealing precipitates were found to grow into faceted shape coherent with the disordered matrix. After prolonged annealing for over 150 h the Ni4W precipitates began to lose coherency by the generation of misfit dislocations. The microstructural observations have been compared for the stoichiometric and off-stoichiometric alloys.

Effect of Strain Rate on Ductile-to-Brittle Transition Temperature of a Free-Standing Pt-Aluminide Bond Coat

The ductile-to-brittle transition temperature (DBTT) of a free-standing Pt-aluminide (PtAl) bondcoat was determined using the microtensile testing method and the effect of strain rate variation, in the range 10(-5) to 10(-1) s(-1), on the DBTT studied. The DBTT increased appreciably with the increase in strain rate. The activation energy determined for brittle-to-ductile transition, suggested that such transition is most likely associated with vacancy diffusion. Climb of aOE (c) 100 > dislocations observed in analysis of dislocation structure using a transmission electron microscope (TEM) supported the preceding mechanism.

Optical and electrical properties of hydrogen-passivated gallium antimonide

The effect of hydrogen-plasma passivation on the optical and electrical properties of gallium antimonide bulk single crystals is presented. Fundamental changes of the radiative recombination after hydrogenation in undoped, zinc-doped, tellurium-doped, and codoped (with Zn and Te) GaSb are reported. The results of optical measurements indicate that passivation of acceptors is more efficient than that of the donors and, in general, the passivation efficiency depends on the doping level. Passivation of deep nonradiative centers is reflected by the gain of photoluminescence intensity and decrease in deep-level transient spectroscopy peak height. Extended defects like grain boundaries and dislocations have also been found to be passivated. The thermal stability of the passivated deep level and extended defects is higher than that of the shallow level. The kinetics of thermally released hydrogen in the bulk has been studied by reverse-bias annealing experiments.

Plate-shaped transformation products in zirconium-base alloys

Plate-shaped products resulting from martensitic, diffusional, and mixed mode transformations in zirconium-base alloys are compared. in the present study. These alloys are particularly suitable for the comparison in view of the fact that the lattice correspondence between the parent beta (bcc) and the product alpha (hcp) or gamma-hydride (fct) phases are remarkably similar for different types of transformations. Crystallographic features such as orientation relations, habit planes, and interface structures associated with these transformations have been compared:, with a view toward examining whether the transformation mechanisms have characteristic imprints on these experimental observables. Martensites exhibiting dislocated lath, internally twinned plate, and self-accommodating three-plate cluster morphologies have been encountered in Zr-2.5Nb alloy. Habit planes corresponding to all these morphologies have been found to be consistent with the predictions based on the invariant plane strain (IFS) criterion. Different morphologies have been found to reflect the manner in which the neighboring martensite variants are assembled. Lattice-invariant shears (LISs) for all these cases have been identified to be either {10 (1) over bar 1}(alpha) ((1) over bar 123)(alpha) slip or twinning on (10 (1) over bar 1)(alpha) planes. Widmanstatten alpha precipitates, forming in a step-quenching treatment, have been shown to have a lath morphology, the alpha/beta interface being decorated with a periodic array of (c + a) dislocations at a spacing of 8 to 10 nm. The line vectors of these dislocations are nearly parallel to the invariant lines. The alpha precipitates, forming in the retained beta phase on aging, exhibit an internally twinned structure with a zigzag habit plane. Average habit planes for the morphologies have been found to lie near the {103}(beta) - {113}(beta) poles, which are close to the specific variant of the {112}(beta) plane, which transforms into a prismatic plane of the type {1 (1) over bar 00}(alpha). The crystallography of the formation of the gamma-hydride phase (fct) from both the alpha and beta phases is seen to match the IFS predictions. While the beta-gamma transformation can be treated approximately as a simple shear on the basal plane involving a change in the stacking sequence, the alpha-gamma transformation call be conceptually broken into a alpha --> beta transformation following the Burgers correspondence and the simple beta-gamma shear process. The active eutectoid decomposition in the Zr-Cu system, beta --> alpha + beta', has been described in terms of cooperative growth of the alpha phase from the beta phase through the Burgers correspondence and of the partially ordered beta' (structurally similar to the equilibrium Zr2Cu phase) through an ordering process. Similarities and differences in crystallographic features of these transformations have been discussed. and the importance of the invariant line vector in deciding the geometry of the corresponding habit planes has been pointed out.

Microstructural stability and superplasticity in an electrodeposited nanocrystalline Ni-P alloy

Stabilization of nanocrystalline grain sizes by second phase particles can facilitate superplasticity at high strain rates and/or low temperatures. A metastable single phase nano-Ni-P alloy prepared by electrodeposition, with a grain size of similar to 6 nm, transforms to a nanoduplex structure at T> 673 K, with similar to 4 vol.% Ni3P particles at triple junctions and within Ni grains. The nanoduplex microstructure is reasonably stable up to 777 K, and the growth of Ni grains occurs in a coupled manner with the growth of Ni3P particles such that the ratio of the two mean sizes (Z) is essentially constant. High temperature tests for a grain size of 290 nm reveal superplastic behavior with an optimum elongation to failure of 810% at a strain rate of 7 x 10(-4) s(-1) and a relatively low temperature of 777 K. Superplastic deformation enhances both grain growth and the ratio Z, implying that grain boundary sliding (GBS) significantly influences the microstructural dynamics. Analysis of the deformation processes suggests that superplasticity is associated with GBS controlled by the overcoming of intragranular particles by dislocations, so that deformation is independent of the grain size. The nano-Ni-P alloy exhibits lower ductility than nano-Ni due to concurrent cavitation caused by higher stresses. (C) 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Tensile flow behaviour of 2.25Cr-1Mo ferritic steel base metal and simulated heat affected zone structures of 2.25Cr-1Mo weld joint

Tensile tests in the temperature range 298 to 873 K have been performed on 2.25Cr-1Mo base metal and simulated heat affected zone (HAZ) structures of its weld joint, namely coarse grain bainite, fine grain bainite and intercritical structure. Tensile flow behaviour of all the microstructural conditions could be adequately described by the Hollomon equation (sigma = K-1 epsilon(n1)) at higher (> 623 K) temperatures. Deviation from the Hollomon equation was observed at low strains and lower (< 623 K) temperatures. The Ludwigson modification of Hollomon's equation, sigma = K-1 epsilon(n1) + exp (K-2 + n(2) epsilon), was found to describe the flow curve. In general, the flow parameters n(1), K-1, n(2) and K-2 were found to decrease with increase in temperature except in the intermediate temperature range (423 to 623 K). Peaks/plateaus were observed in their variation with temperature in the intermediate temperature range coinciding with the occurrence of serrated flow in the load-elongation curve. The n(1) Value increased and the K-1 value decreased with the type of microstructure in the order: coarse grain bainite, fine grain bainite, base metal and intercritical structure. The variation of nl with microstructure has been rationalized on the basis of mean free path (MFP) of dislocations which is directly related to the inter-particle spacing. Larger MFP of dislocations lead to higher strain hardening exponents n(1).

Evolution of crystallographic texture during deformation of submicron grain size titanium

Evolution of deformation texture in commercially pure titanium with submicron grain size (SMG) was studied using x-ray diffraction (XRD) and electron back scatter diffraction (EBSD) methods. The material was deformed by rolling at room temperature. The deformation mechanism was found to be slip dominated with a pyramidal slip system facilitating plastic deformation. No evidence of tensile or compressive twinning was detected, as generally seen in the case of titanium with conventional microcrystalline grain size. The absence of twinning and the propensity of the pyramidal slip system in the SMG Ti is attributed to the lack of coordinated motion of zonal partial dislocations that leads to twinning.

Effect of irradiation on the microstructure and mechanical behavior of nanocrystalline nickel

The effect of 4.0 MeV proton irradiation on the microstructure and mechanical properties of nanocrystalline (nc) nickel was investigated. The irradiation damage induced in the sample was of the order of 0.004 dpa. Transmission electron microscopy of irradiated samples indicated the presence of dislocation loops within the grains. An increase in hardness and strain-rate sensitivity (m) of nc-Ni with irradiation was noted. The rate-controlling deformation mechanism in irradiated nc-Ni was identified to be interaction of dislocations with irradiation-induced defects. (C) 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Nanostructure of giant magnetoresistive oxide film Nd2/3Sr1/3MnO3 by scanning tunneling microscopy

Scanning tunneling microscopy was used to study the surface nanostructure of the epitaxial film Nd2/3Sr1/3MnO3 that shows giant magnetoresistance. The surface morphology of the film consists of a number of overlapping platelets of about 30–35 Å diameter that grow at an angle of 35°–45° to the surface normal. The peak to peak height of the platelets are multiples of the c‐axis lattice parameter of 7.85 Å showing that the growth of the platelets takes place by the layer by layer addition of one formula unit. The mean surface roughness is about 10 Å. In the range of a few microns the film exhibits no defects or dislocations. The film is unstable in ambient atmosphere and tends to get covered by an adsorbate layer. Tip‐surface interactions cause the adsorbate to be dislodged exposing the surface nanostructure. The degradation of the film in real time when imaged in air was recorded. The adsorbates increase the surface roughness of the film.