Effects of temper level on the dependence of fatigue crack growth threshold and crack closure on the prior austenitic grain size

An attempt has been made to systematically investigate the effects of microstructural parameters, such as the prior austenite grain size (PAGS), in influencing the resistance to fatigue crack growth (FCG) in the near-threshold region under three different temper levels in a quenched and tempered high-strength steel. By austenitizing at various temperatures, the PAGS was varied from about 0.7 to 96 μm. The microstructures with these grain sizes were tempered at 200 °C, 400 °C, and 530 °C and tested for fatigue thresholds and crack closure. It has been found that, in general, three different trends in the dependence of both the total threshold stress intensity range, ΔK th , and the intrinsic threshold stress intensity range, ΔK eff, th , on the PAGS are observable. By considering in detail the factors such as cyclic stress-strain behavior, environmental effects on FCG, and embrittlement during tempering, the present observations could be rationalized. The strong dependence of ΔK th and ΔK eff, th on PAGS in microstructures tempered at 530 °C has been primarily attributed to cyclic softening and thereby the strong interaction of the crack tip deformation field with the grain boundary. On the other hand, a less strong dependence of ΔK th and ΔK eff, th on PAGS is suggested to be caused by the cyclic hardening behavior of lightly tempered microstructures occurring in 200 °C temper. In both microstructures, crack closure influenced near-threshold FCG (NTFCG) to a significant extent, and its magnitude was large at large grain sizes. Microstructures tempered at the intermediate temperatures failed to show a systematic variation of ΔKth and ΔKeff, th with PAGS. The mechanisms of intergranular fracture vary between grain sizes in this temper. A transition from “microstructure-sensitive” to “microstructure-insensitive” crack growth has been found to occur when the zone of cyclic deformation at the crack tip becomes more or less equal to PAGS. Detailed observations on fracture morphology and crack paths corroborate the grain size effects on fatigue thresholds and crack closure.

A Convenient High-Yield Room-Temerature Synthesis of Mixed Tri(Amino) Silanes by Transmination of Tris(Dicyclohexylamino) Silane And-Their Characterization

Tris(dicyclohexylamino)silane. (DCA)3SiH. is prepared by the reaction of trichlorosilane with dicyclohexylamine. This is found to undergo transamination reactions with other secondary amines (R2NH). such as pyrrolidine, piperidine, hexamethyleneimine. morpholine. N-methylpiperazine and diethylamine to yield mixed tri(amino)silanes of the formula (DCA)(R2N)2SiH in quantitative yields. These new derivatives are found to be moisture sensitive and hydrolyze to yield their respective amines, hydrogen and silica. They are found to be stable in an inert atmosphere. They have been characterized by IR, NMR (H-1, Si-29), mass spectroscopy and CHN analysis. N-15 NMR for one of the compounds has been done.

Grain size effect on the phase transformation temperature of nanostructured CuFe2O4

We report a large decrease in tetragonal to cubic phase transformation temperature when grain size of bulk CuFe2O4 is reduced by mechanical ball milling. The change in phase transformation temperature was inferred from in situ high temperature conductivity and x-ray diffraction measurements. The decrease in conductivity with grain size suggests that ball milling has not induced any oxygen vacancy while the role of cation distribution in the observed decrease in phase transformation temperature is ruled out from in-field Fe-57 Mossbauer and extended x-ray absorption fine structure measurements. The reduction in the phase transformation temperature is attributed to the stability of structures with higher crystal symmetry at lower grain sizes due to negative pressure effect. (C) 2011 American Institute of Physics. doi: 10.1063/1.3493244]

Creep in TiO2 doped Zirconia: Implications for high strain rate superplasticity

In ceramics, dopants offer the possibility of higher creep rates by enhancing diffusion. The present study examines the potential for high strain rate superplasticity in a TiO2 doped zirconia, by conducting creep experiments together with microstructural characterization. It is shown that both pure and doped zirconia exhibit transitions in creep behaviour from Coble diffusion creep with n similar to 1 to an interface controlled process with n similar to 2. Doping with TiO2 enhances the creep rate by over an order of magnitude. There is evidence of substantial grain boundary sliding, consistent with diffusion creep.

High Yield Room Temperature Synthesis And Spectral Studies Of Tri(Amino)Silanes: (R2n)3SIH

Tri(amino)silanes were prepared by the condensation of trichlorosilane with secondary amines in 1:6 molar ratio. Reactions of trichlorosilane with pyrrolidine, piperidine, hexamethyleneimine, morpholine, N-methylpiperazine and diethylamine afford the tri(amino)silanes in nearly quantitative yields. Their physical and spectroscopic properties are discussed. All these compounds are highly sensitive to moisture and hydrolyse to silica and the respective amine with the evolution of hydrogen. The compounds have been characterised by IR, 1H NMR, [1H]29Si NMR spectroscopic methods and CHN elemental analysis.

Effect of strain rate on the high-temperature low-cycle fatigue properties of a nimonic PE-16 superalloy

Strain-rate effects on the low-cycle fatigue (LCF) behavior of a NIMONIC PE-16 superalloy have been evaluated in the temperature range of 523 to 923 K. Total-strain-controlled fatigue tests were per-formed at a strain amplitude of +/-0.6 pct on samples possessing two different prior microstructures: microstructure A, in the solution-annealed condition (free of gamma' and carbides); and microstructure B, in a double-aged condition with gamma' of 18-nm diameter and M23C6 carbides. The cyclic stress response behavior of the alloy was found to depend on the prior microstructure, testing temperature, and strain rate. A softening regime was found to be associated with shearing of ordered gamma' that were either formed during testing or present in the prior microstructure. Various manifestations of dynamic strain aging (DSA) included negative strain rate-stress response, serrations on the stress-strain hysteresis loops, and increased work-hardening rate. The calculated activation energy matched well with that for self-diffusion of Al and Ti in the matrix. Fatigue life increased with an increase in strain rate from 3 x 10(-5) to 3 x 10(-3) s-1, but decreased with further increases in strain rate. At 723 and 823 K and low strain rates, DSA influenced the deformation and fracture behavior of the alloy. Dynamic strain aging increased the strain localization in planar slip bands, and impingement of these bands caused internal grain-boundary cracks and reduced fatigue life. However, at 923 K and low strain rates, fatigue crack initiation and propagation were accelerated by high-temperature oxidation, and the reduced fatigue life was attributed to oxidation-fatigue interaction. Fatigue life was maximum at the intermediate strain rates, where strain localization was lower. Strain localization as a function of strain rate and temperature was quantified by optical and scanning electron microscopy and correlated with fatigue life.

Metastable extension of the fluorite phase field in Y2O3---ZrO2 and its effect on grain growth

Pure Y2O3 and Y2O3---ZrO2 solid solutions have been prepared by melt atomization and by pyrolysis of nitrate solutions. Extended solubility is readily achieved in both techniques for the entire composition range investigated: melts with 0–30% ZrO2 and precursors with 0–50% ZrO2. However, solidification of under cooled droplets yields almost exclusively single phase powders with the structure of cubic yttria (D53). In contrast, the pyrolysis route leads to a sequence of metastable microstructures beginning with a nanocrystalline disordered fluorite-based (C1) solid solution. Further heating leads to the evolution of much larger (micron size) flake crystals with a {001} texture, concurrent with partial ordering of the oxygen ions to the sites occupied in the D53 structure. The driving force for ordering and the rate of grain growth decrease with increasing ZrO2 addition. Abrupt heating to high temperatures or electron irradiation can induce ordering without substantial grain growth. There is no significant reduction in porosity during the recrystallization, which with the other observations suggests that grain growth is driven by the free energy available for the ordering transformation from fluorite to the yttria structure. This route offers opportunities for single crystal thin film development at relatively low processing temperatures.

Metastable extension of the fluorite phase field in Y2O3---ZrO2 and its effect on grain growth

Pure Y2O3 and Y2O3-ZrO2 solid solutions have been prepared by melt atomization and by pyrolysis of nitrate solutions. Extended solubility is readily achieved in both techniques for the entire composition range investigated: melts with 0-30% ZrO2 and precursors with 0-50% ZrO2. However, solidification of under cooled droplets yields almost exclusively single phase powders with the structure of cubic yttria (D5(3)). In contrast, the pyrolysis route leads to a sequence of metastable microstructures beginning with a nanocrystalline disordered fluorite-based (C1) solid solution. Further heating leads to the evolution of much larger (micron size) flake crystals with a {001} texture, concurrent with partial ordering of the oxygen ions to the sites occupied in the D5(3) structure. The driving force for ordering and the rate of grain growth decrease with increasing ZrO2 addition. Abrupt heating to high temperatures or electron irradiation can induce ordering without substantial grain growth. There is no significant reduction in porosity during the recrystallization, which with the other observations suggests that grain growth is driven by the free energy available for the ordering transformation from fluorite to the yttria structure. This route offers opportunities for single crystal thin film development at relatively low processing temperatures.

Influence of grain boundary sliding on diffusion in yttria doped zirconia

Grain boundary sliding during high temperature deformation can lead to stress concentrations and an enhancement of diffusion in mobile boundaries. Experiments were conducted on a fine grained 3 mol% yttria stabilized tetragonal zirconia, under conditions associated with superplastic flow involving grain boundary sliding. Tracer diffusion studies under creep conditions and without load indicate that there is no enhancement in either the lattice or grain boundary diffusivities. The experimental creep data are consistent with an interface controlled diffusion creep mechanism. (C) 2011 Elsevier Ltd. All rights reserved.

Radiation induced modifications on microstructure and related properties of high temperature superconductor YBCO

Role of swift heavy ion irradiation on the modification of transport and structural properties of high temperature superconductors is studied. Good quality YBCO thin films prepared by high pressure oxygen sputtering and laser ablation were used in this investigation. Resistivity and atomic force microscopy (AFM) were mainly used to probe superconducting and microstructural modifications resulted from the irradiation of high energy and heavy ions like 100 MeV oxygen and 200 MeV silver. Radiation induced sputtering or erosion is likely to be a major disastrous component of such high energy irradiation that could be powerful in masking phase coherence effects, atleast in grain boundaries. The extent of damage/nature of defects other than columnar defects produced by swift heavy ions is discussed in the light of AFM measurements. The effect of high energy oxygen ion irradiation is anomalous. A clear annealing effect at higher doses is seen. (C) 1999 Elsevier Science B.V. All rights reserved.

Investigation of Surface Grooves from Migrating Grain Boundaries

Visible-light microscopy (VLM) and atomic-force microscopy (AFM) were used to study the progression of grain-boundary grooving and migration in high-purity alumina (Lucalox™). Groove profiles from the same grain boundaries were revisited using AFM following successive heat-treatments. The grooves measured from migrating grain boundaries were found to have asymmetric partial-angles compared to those measured from boundaries that did not migrate during the experiment. For a moving boundary, the grain with the larger partial-angle was consistently found to grow into the grain with the smaller partial-angle. Migrating boundaries were observed to leave behind remnant thermal grooves. The observations indicate that the boundary may be bowing out during the migration process.

Effect of spinel second phase on high temperature deformation in alumina

Constant stress compression creep experiments were carried out on high purity alumina composites with spinel contents of 8 and 30%, corresponding to a situation with isolated and interconnected second phases. The creep experiments were conducted over a stress and temperature range of 10 to 150 MPa and 1623 to 1723 K, respectively. Analysis of the experimental data indicated that the variation in spinel content did not have any influence on high temperature deformation in the composite. The spinel phase retards grain growth, and this may enhance superplasticity in alumina-spinel composites.

High-temperature deformation processing maps for a NiTiCu shape memory alloy

The properties of widely used Ni-Ti-based shape memory alloys (SMAs) are highly sensitive to the underlying microstructure. Hence, controlling the evolution of microstructure during high-temperature deformation becomes important. In this article, the ``processing maps'' approach is utilized to identify the combination of temperature and strain rate for thermomechanical processing of a Ni(42)Ti(50)Cu(8) SMA. Uniaxial compression experiments were conducted in the temperature range of 800-1050 degrees C and at strain rate range of 10(-3) and 10(2) s(-1). Two-dimensional power dissipation efficiency and instability maps have been generated and various deformation mechanisms, which operate in different temperature and strain rate regimes, were identified with the aid of the maps and complementary microstructural analysis of the deformed specimens. Results show that the safe window for industrial processing of this alloy is in the range of 800-850 degrees C and at 0.1 s(-1), which leads to grain refinement and strain-free grains. Regions of the instability were identified, which result in strained microstructure, which in turn can affect the performance of the SMA.

Evolution of texture and grain boundary microstructure in two-phase (α + β) brass during recrystallization

The evolution of texture and microstructure during recrystallization is studied for two-phase copper alloy (Cu–40Zn) with a variation of the initial texture and microstructure (hot rolled and solution treated) as well as the mode of rolling (deformation path: uni-directional rolling and cross rolling). The results of bulk texture have been supported by micro-texture and microstructure studies carried out using electron back scatter diffraction (EBSD). The initial microstructural condition as well as the mode of rolling has been found to alter the recrystallization texture and microstructure. The uni-directionally rolled samples showed a strong Goss and BR {236}385 component while a weaker texture similar to that of rolling evolved for the cross-rolled samples in the α phase on recrystallization. The recrystallization texture of the β phase was similar to that of the rolling texture with discontinuous 101 α and {111} γ fiber with high intensity at {111}101. For a given microstructure, the cross-rolled samples showed a higher fraction of coincident site lattice Σ3 twin boundaries in the α phase. The higher fraction of Σ3 boundaries is explained on the basis of the higher propensity of growth accidents during annealing of the cross-rolled samples. The present investigation demonstrates that change in strain path, as introduced during cross-rolling, could be a viable tool for grain boundary engineering of low SFE fcc materials.

Texture evolution in high strain rate deformed Cu-10Zn alloy

High strain rate deformation behavior of Cu-10Zn alloy was studied. A weak texture with fine grain size was observed at high strain rate. The weak texture has been attributed to activity of higher number of slip systems under dynamic loading conditions. Twinning has minimal role on texture. (C) 2012 Elsevier B.V. All rights reserved.