Effect of iron and silicon on structure transformations and on microhardness of Al-30 wt. % Zn alloy aged at 90 °C

The structure transformations during the ageing at 90 C of Al-30 wt. % Zn alloys prepared from Al of 99.7, 99.99 and 99.999 wt. % were studied by X-ray diffraction and by transmission electron microscopy. Simultaneously, the measurement of Vicker's microhardness was carried out. It was found that Fe and Si impurities affect substantially the structure transformations and the microhardness values during the ageing process. These impurities retard the formation of lamellar aggregates of-phase and of impoverished-matrix and thus they slow down the softening of the alloy.In conclusion we would like to express our thanks to Doc. Dr. V.Syneek CSc. for his valuable discussions. We are also indebted to Mr. V.Petr and Mr. Z.iký for their help in the microhardness and X-ray diffraction measurements, and to Mr. P.Vyhlídka for the homogeneity check of the investigated samples.     

Effect of plastic deformation on precipitation in Al-30 wt.% Zn alloy aged at 200 °C

The electron microscopic investigation of an Al-30 wt.% Zn alloy reveals that the plastic deformation of quenched samples substantionally modifies the phase transformation processes examined in the alloy aged at 200°C. Whereas the growth kinetics of metastable precipitates and associated solute diffusion are unaffected by cold rolling the alloy specimens from 9% up to 97·5% reduction in thickness, the rate of all observed transformations is enhanced considerably by prior plastic deformation. A corresponding increase of stored strain energy within the lattice provides namely an additional driving force for the establishment of a new precipitate/matrix interface of higher surface energy on the transformation of a metastable precipitate into a more stable one. The sizes of transforming transition precipitates consequently diminish with an increase of cold work and the respective transformations are thus accelerated.High dislocation density in heavily cold worked alloy also reduces the nucleation barrier for a heterogeneous nucleation on dislocations. The formation of platelike coherent_coh precipitates with internal cubic structure on dislocations is observed followed by the transformation of_coh into spheroidical semicoherent precipitates. The non-uniform distribution of stresses and strains in cold rolled specimens leads to the development of deformation bands in the higher strained regions of even lightly deformed alloy. The direct precipitation of equilibrium precipitates in deformation bands is already observed immediately after cold work analogously to the -allotriomorph formation at grain boundaries.     

Precipitation sequences and transformation kinetics in the Al-30 wt.% Zn alloy aged below 160°C

The transformation sequences in the Al-30 wt.% Zn alloy aged below 160 °C have been investigated by X-ray diffraction and transmission electron microscopy. The sequence G.-P. zones _R has been observed between 85 and 161 °C, whereas the direct G.-P. zones to-transformation occurs below 85 °C. The identical isothermal growth kinetics of both the G.-P. zones and the _R -precipitates was found. The log-log plots yielding a set of parallel straight lines from 50 to 150 °C indicate no change in the activation energy of growth of both these precipitates. The change in the precipitation sequence led to the change in the transformation kinetics. The T-T-T curves have been measured for the formation of metastable _R -phase and for the completion of ellipsoidal G.-P. zones or of _R to-transformation. The retardation in reaching equilibrium found below 85 °C was associated with the observed change in the transformation sequence. This was explained by the different accommodation of the misfit at the interfaces between G.-P. zones or _R -precipitates and the-matrix.The authors are much indebted to Doc. Dr. V.Syneek, CSc. for stimulating discussions. Our thanks are also due to Ing. V.íma and Mr. P.Vyhlídka for the preparation and careful chemical analyses of the investigated samples. The assistance of Mr. Z.iký and Mr. V.Petr in X-ray diffraction measurements and the heat-treatment of samples is appreciated.     

The influence of the α′-precipitates on the electrical conductivity of Al-21·8 AT. % Zn alloy at higher temperatures

The applicability of the classical theoretical formulae for electrical conductivity of disperse metallic systems was experimentally verified on the Al-21·8 at. % Zn alloy. This alloy represents a two-phase system in the investigated temperature interval 276–302 °C. The conductivity values calculated for the system consisting of discrete spheres randomly distributed within the continuous matrix were compared with the measured isothermal deviationsR _f from the ideal resistivity, corresponding to the hypothetical continuous solid solution at the same temperature. The temperature 308 °C for the stable solvus was derived by extrapolation ofR _f s values.I would like to express my thanks to Doc. Dr. V.Syneek CSc., for stimulating author's interest in this problem and for providing helpful discussions. The author is indebted to Mrs.Mendlová for careful evaluation of experimental data.     

Initiation of discontinuous precipitation at interphase boundaries in a two-phase Zn–6.3 at.% Ag alloy

Discontinuous precipitation (DP) was found to initiate at both η′–ε interphase and η′–η′ grain boundaries in a two-phase Zn–6.3?at.%?Ag alloy consisting of ε and supersaturated η′ phases. The η′–ε interphase boundaries at which DP has initiated illustrated a sinusoidal interface during ageing, which implies that the morphological instability is a prerequisite for the DP initiation at an η′–ε interphase boundary. The application of the morphological instability model for solid–solid interfaces has indicated that the interface protuberances grow into the supersaturated η′ and the interphase boundary becomes unstable since the observed wavelength of serrated η′–ε interphase boundaries was larger than the critical value predicted by the model. A solute-depleted region is therefore established in front of the η′–ε interphase boundary, which provides an appropriate site leading to a DP reaction. Based on this, a nucleation mechanism of DP at the interphase boundaries is proposed accordingly: the allotriomorphs of DP can be directly developed from ε protuberances of a serrated interphase boundary.     

A resistometric investigation of the decomposition kinetics of Al-21·8 at.% Zn solid solution at 276 °C

Under the condition of nearly equilibrium concentration of vacancies, time dependence of the amount of isothermal transformation given byy=R/R _f was investigated whereR _f is the total structural change of resistivity on completion of the whole process andR is the measured resistivity change. The investigation was done on the 21·8 at.% (40·3wt.%) Zn alloy under the condition of relatively low supersaturation of a few degrees centigrade below the metastable _R solvus line. The total transformation involves four kinetic stages: the first two stages correspond probably to diffusion-controlled growth of the _R particles from the supersaturated solid solution and to the ripening of these particles till their conversion to the cubic phase takes place. The last two kinetic stages account analogously for the particles growth and ripening. Both _R and phases were identified by the transmission electron microscopy. When separating the individual stages, the approximation byy=1–exp [–(mt) ⁿ] of the amount of transformationy was used. The approximation allowed to get the starting values of both the time and the change of the structural part of the electrical resistance for individual stages and also to derive the parametersm _i, n_i which had to be redetermined for the individual separated stages. These data made it possible to synthetize the experimental curves ofR andy vs. time for the total transformation.It is a pleasure to thank Doc. Dr. V.Syneek CSc. for stimulating the author's interest in this problem and for providing helpful discussions. I also would like to express my thanks to Ing. P.Bartuka CSc. for the transmission electron microscopic study carried out to identify the particular phases. The author is indebted to Ing.V. íma for the preparation of the investigated alloy and to Mrs. A.Mendlová and Mr. P.Vyhlídka for technical assistance.     

The effect of Zn on precipitation in Al–Mg–Si alloys

Effects of addition of Zn (up to 1 wt%) on microstructure, precipitate structure and intergranular corrosion (IGC) in an Al–Mg–Si alloys were investigated. During ageing at 185?°C, the alloys showed modest increases in hardness as function of Zn content, corresponding to increased number densities of needle-shaped precipitates in the Al–Mg–Si alloy system. No precipitates of the Al–Zn–Mg alloy system were found. Using high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), the Zn atoms were incorporated in the precipitate structures at different atomic sites with various atomic column occupancies. Zn atoms segregated along grain boundaries, forming continuous film. It correlates to high IGC susceptibility when Zn concentration is ~1wt% and the materials in peak-aged condition.     

Effect of external stress on discontinuous precipitation in a Cu–2.1 wt % Be alloy

The influence of an applied stress on discontinuous precipitation (DP) in a Cu–2.1 wt % Be alloy aged at 300°C was examined. A compressive stress accelerates the growth of DP cells, which consist of lamellae of the precipitated γ phase and the solute-depleted α phase, but a tensile stress does not essentially change it. The cell growth rates along the loading direction under the compressive and tensile stress are identical to those along the direction perpendicular to the loading direction under the same stress. Both the compressive and tensile stresses have no influence on the incubation time to initiate DP. From measurements of the specimen length change and investigations of the distribution of γ variants in cells in a particular case, specific γ variants among crystallographically equivalent ones are found to be formed, depending on the sense of the applied stress. This result, together with the dependence of the cell growth rate on the sense of the applied stress, can be well understood through the interaction energy between the external stress and the misfit strains of discontinuous γ precipitates.     

Decomposition of an Fe-Cr 38 wt.% chromium stainless steel at 475 °C

The physical changes occurring at 475 °C in an Nb and Al stabilized stainless steel containing 38 wt.% Cr have been studied by Mössbauer spectroscopy. The specimen started to decompose when held at 475 °C. Decomposition still continues after 500 hours into a paramagnetic Cr-rich -phase and a nearly pure Fe -phase. The magnetic field distribution of the initial sample indicates that considerable decomposition has already taken place into an -phase with an estimated 15 at.% iron, and an iron-rich -phase with an estimated 18 at.% Cr.     

The effect of vacuum annealing on the remediation abilities of iron and iron−nickel nanoparticles

Zero-valent iron nanoparticles are effective remediators of uranium from solution. It is postulated that the improved core crystallinity and the migration of impurity phases to the nanoparticle surfaces induced by annealing may improve their corrosion resistance and reactive lifespan. The ability of annealed and non-annealed Fe and FeNi nanoparticles to remediate a U-contaminated effluent from AWE, Aldermaston was investigated. Nanoparticles (of diameter typically between 0 and 100 nm) were introduced to the effluent and allowed to react for 7 days during which the liquid and nanoparticulate solids were periodically sampled. In all the systems, the maximum U-uptake occurred within 1 h of introduction, with variable efficiency. The Fe nanoparticles removed 98% of the total U from solution, resulting in a final U-concentration of <4 μg/L. A rapid release of Fe into solution was recorded early in the reaction period: attributed to limited partial dissolution of the nanoparticles. Annealing the Fe nanoparticles did not affect their efficiency but the dissolution of Fe was significantly reduced and X-ray Photoelectron Spectroscopy indicated slower progressive oxidation. The performance of the FeNi nanoparticles was significantly improved by annealing, with U-uptake increasing from 50 to 94%. Although the dissolution of Ni was completely inhibited by annealing, the Fe dissolution increased compared to that observed for the non-annealed FeNi nanoparticles, in contrast to behaviour exhibited by Fe-annealed nanoparticles. In all the systems, U was reduced to U(IV) and retained on the surfaces of the nanoparticulate solids for up to 48 h; the U-stability was not affected by annealing the Fe or the FeNi nanoparticles before use.     

Study on the effect of Ar9+ ion irradiation of Zr–2.5 wt.% Nb alloy pressure tube

Response of Zr–2.5 wt.% Nb alloy pressure tube, used in PHWR nuclear reactors, to 315 keV Ar⁹⁺ ion irradiation at room temperature was investigated in the fluence range of 3.1?×?10¹⁵–4.17?×?10¹⁶ Ar⁹⁺?cm^?2. Changes in microstructural parameters, viz., the size of coherently scattering domains, microstrain and dislocation density, upon irradiation were ascertained through grazing incidence X-ray diffraction. In general, a decrease in domain size was observed with fluence with a corresponding increase in microstrain and dislocation density. Residual stress measurement showed the development of compressive stresses in place of tensile after irradiation. Transmission electron microscopy showed the formation of dislocation loops of ?a?-type and ?c?-type during irradiation. The hardness of irradiated samples, probed through nanoindentation technique, was found to be higher in comparison with unirradiated samples. The above findings have been rationalised on the basis of the defects generated during the Ar⁹⁺ ion irradiation.     

The nitrogen-absorption isotherm for Fe–21.5 at. % Cr alloy: dependence of excess nitrogen uptake on precipitation morphology

Nitriding of Fe–21.5 at. % Cr alloy leads to a “discontinuously coarsened”, chromium-nitride/ferrite lamellar precipitation morphology in the nitrided zone. The nitrogen-absorption isotherm for this alloy with this precipitation morphology was determined at 560°C. To assure a constant precipitation morphology the Fe–21.5 at. % Cr specimen was first homogeneously pre-nitrided (at 580°C in an ammonia/hydrogen gas mixture of nitriding potential 0.103 atm^?1/2) and then de-nitrided (at 470°C in hydrogen gas atmosphere). The amount of nitrogen remaining in the de-nitrided specimen indicated that the composition of the nitride precipitates is CrN and not (Fe, Cr)N. The measured nitrogen-absorption isotherm revealed the presence of excess nitrogen in the nitrided specimen, which is a surprise in view of the coarse, lamellar precipitation morphology. The occurrence of this excess nitrogen could be ascribed to an unexpected, minor fraction of the total chromium content in the alloy present as coherent, tiny nitride platelets within the ferrite lamellae of the “discontinuously coarsened” lamellar precipitation morphology, as evidenced by transmission electron microscopy. A possible kinetic background for this unusual phenomenon was discussed.     

Superplasticity in A Zn-1·1 wt.% Al alloy III. The influence of grain size

The paper represents the third instalment of the series dealing with the superplastic deformation in a Zn-1·1 wt. % Al alloy and is devoted to the influence of grain size on the deformation behaviour of this alloy. Deformation characteristics were measured at two temperatures — 293 and 500 K. The grain size dependence of the flow stress observed was found opposite to that predicted by the Hall-Petch relation. Such a behaviour was explained under the assumption that grain boundaries might act as sites of rapid recovery of lattice dislocations. The results obtained at temperature 293 K proved that the transition between the regions of abnormal behaviour (with the flow stress increasing with increasing grain size) and normal behaviour (with the flow stress decreasing with increasing grain size) was not directly connected with the transition from the superplastic to the nonsuperplastic state. The results obtained at 500 K revealed dynamic recrystallization and a grain refinement in samples with initially coarser structures. Such a change in grain structure was accompanied with a development of superplastic characteristics.     

Precipitation structure in an Al-2·0 at. % Zn-1·0 at. % Mg alloy within and close to the grain boundaries and its effects on mechanical properties

During ageing the Al-2·0 at. %Zn-1·0 at. % Mg alloy at elevated temperatures the width of the precipitation free zone (PFZ) at both sides of the grain boundaries (GB) is identical with that free of quenched-in dislocation loops (DL). After sufficiently long ageing a band of precipitates is growing inside the former PFZ and the DLs in the midgrain regions act as sites for the heterogeneous nucleation of the-phase. Two precipitation processes significantly affect the mechanical properties. TEM correlates grain boundary precipitate density and morphology with grain boundary misorientation.     

The effect of laser surface treatment of Al-Si alloy on the surface hardness and structure

In this paper, some samples of Al-Si alloy with various silicon content were treated by laser beam. The effects on structure, hardness and substructure of samples were investigated. The experimental results show that the primary crystal Al and eutectic silicon in the laser treated samples is got thinning obviously, the mosaic dimension is decreased and the dislocation density is increased.     

Effect of cooling speed on structure and properties of rapidly solidified Pb–25wt.% Sn alloy

The effect of cooling speed on structure, hardness, mechanical and electrical transport properties of rapidly solidified Pb–25wt.% Sn alloy have been investigated. A single roller melt spinning technique with linear speeds 15.7 and 31.7 m/s, was used for the preparation of specimens. The results showed that a lower cooling speed increased the precipitation of Sn in a Pb-matrix phase as compared with the higher cooling speed. This decomposition behavior decreased the electrical resistivity and increased the internal friction, thermal diffusivity and Vickers microhardness of the lower cooling speed as compared with those of the higher cooling speed.     

Examination of the distribution of the tensile deformation systems in tension and tension-creep of Ti-6Al-4V (wt.%) at 296 K and 728 K

The deformation behaviour of an α + β Ti–6Al–4V (wt.%) alloy was investigated during in situ deformation inside a scanning electron microscopy (SEM). Tensile experiments were performed at 296 and 728 K (~0.4Tm), while a tensile-creep experiment was performed at 728 K and 310 MPa (σ/σ_ys = 0.74). The active deformation systems were identified using electron backscattered diffraction-based slip-trace analysis and SEM images of the specimen surface. The distribution of the active deformation systems varied as a function of temperature. Basal slip deformation played a major role in the tensile deformation behaviour, and the relative activity of basal slip increased with increasing temperature. For the 296 K tension deformation, basal slip was less active than prismatic slip, whereas this was reversed at 728 K. Twinning was observed in both the 296 and 728 K tension experiments; however, no more than 4% of the total deformation systems observed was twins. The tension-creep experiment revealed no slip traces, however grain boundary ledge formation was observed, suggesting that grain boundary sliding was an active deformation mechanism. The results of this work were compared with those from previous studies on commercially pure Ti, Ti–5Al–2.5Sn (wt.%) and Ti–8Al–1Mo–1V (wt.%), and the effects of alloying on the deformation behaviour are discussed. The relative amount of basal slip activity increased with increasing Al content.     

Effect of dissolution of Θ-phase on characteristic parameters of work-hardening in AL-2·5wt. % Cu alloy

Stress-strain curves of slowly cooled and quenched Al-2·5 wt. % Cu alloy were studied in the temperature range 693 K to 773 K. The linear work-hardening coefficient, the fracture time, the yield stress and the fracture stress of annealed and quenched samples decreased with increasing deformation temperature and exhibited a minimum at 733 K. The X-ray analysis of the slowly cooled and quenched samples showed that the lattice parametera of Al-matrix and the ratioc/a of the tetragonal -phase reached a minimum and a maximum value, respectively, at the dissolution temperature.     

The effect of Cu on precipitation in Al–Mg–Si alloys

TEM investigations of two alloys isothermally heat treated at 175°C and 260°C show how Cu additions to the Al–Mg–Si system affect precipitation. Both alloys had a solute content Mg?+?Si?=?1.3 at.%, 0.127 at.% Cu, but with Mg/Si 0.8 and 1.25. Cu-containing Guinier-Preston (GP) zones and three types of Q′ precursors are identified as most common phases at peak-hardness conditions, whereas β″ accounts for maximum 30% of the total number of precipitates. The precursors have needle (L and S precipitates) or plate (C precipitate) morphologies. They consist of different arrangements of Al, Mg and Cu atoms on a grid defined by triangularly arranged Si planes parallel with and having the same period as {100} Al planes. The Si grid is composed of nearly hexagonal sub-cells of a?=?b?=?4.05?Å, c?=?4.05?Å. The Cu arrangement on the grid is often disordered in the needle precursors. The plate precursor is ordered, with a monoclinic unit cell of a?=?10.32?Å, b?=?8.1?Å, c?=?4.05?Å, γ?=?101°.     

An effect of oxygen content on electrical properties of donor centres formed in cz-silicon at 600°C

Electrical properties of oxygen-related donors formed in Cz-Si at 600°C are investigated. The formation of these donors was found to be very sensitive to the oxygen concentration. Electrical measurements on heat-treated and irradiated samples made it possible to outline the distribution of single and double donors over their ionization energies. A similarity in electrical properties of oxygen-related donors formed in Cz-Si at 450° and 600°C is discussed.