Elevated temperature directional recrystallization of high-purity nickel

Electron backscattered diffraction has been used to characterise the three different kinds of boundaries that occur in grains that are generated by secondary recrystallization during directional annealing of high-purity nickel. Boundaries between columnar grains (CC boundaries) can be twin boundaries, low-angle boundaries or high-angle grain boundaries. The frequency of low-angle CC boundaries dropped from 25% to 0% while the frequency of the high-angle CC boundaries increased from 19% to 67% when the annealing temperature was increased from 1000°C to 1200°C. The misorientation angles of boundaries between columnar grains and small equiaxed grains ahead of them (CE boundaries) was random at 1200°C but had a 40° rotation relationship about ?111? at 1000°C. It was found out that the character of the CC boundaries is determined by relative mobility of the CE boundaries, which is determined by the processing temperature rather than the energy of the CC boundaries themselves. The character of the island grain boundaries sometimes found with columnar grains was not affected by the annealing temperature or the drawing velocity.     

Texture evolution in Mg–Mn and Mg–Mn–Ce alloys and the effect of as-cast grain size

Texture evolution in rolled (400°C) and annealed (450°C) Mg–1% Mn-based alloys containing different levels of Ce was examined. It was found that Ce refines the as-cast and rolled/annealed grain structure. The overall intensity of the basal texture decreases with Ce additions in both the rolled and subsequently annealed condition. A strong relationship was found between maximum intensity (M) of rolling and annealing textures and the as-cast effective grain size, d?′, i.e. M?∝?e^{0.4 d ?′} (R ^2?=?0.8), which was attributed to the role of plastic compatibility stresses which lead to grain boundary deformation altering the balance of deformation modes. Contributions from Ce solute effects and lattice parameter changes are also discussed.     

Crystal microstructure of annealed nanocrystalline Chromium studied by synchrotron radiation diffraction

The microstructure of electrodeposited nanocrystalline chromium (n-Cr) was studied by using synchrotron radiation (SR) diffraction, SEM, TEM, and EDX techniques. The as-prepared n-Cr samples show the standard bcc crystal structure of Cr with volume-averaged column lengths varying from 25 to 30 nm. The grain growth kinetics and the oxidation kinetics were studied by time resolved SR diffraction measurements with n-Cr samples annealed at 400, 600, and 800 °C. The grain growth process is relatively fast and it occurs within the first 10 min of annealing. The final crystallite size depends only on the annealing temperature and not on the initial grain size or on the oxygen content. The final volume-averaged column lengths observed after 50 min annealing are 40(4), 80(1), and 120(2) nm for temperatures 400, 600, and 800 °C, respectively. It is shown that annealing ex situ of n-Cr at 800 °C both under vacuum and in air gives a grain growth process with the same final crystallite sizes. The formation of the Cr₂O₃ and CrH phases is observed during annealing.     

Synthesis of nano-polycrystalline diamond from glassy carbon at pressures up to 25 GPa

ABSTRACT

Nano-polycrystalline diamond (NPD) with various grain sizes has been synthesized from glassy carbon at pressures 15–25?GPa and temperatures 1700–2300°C using multianvil apparatus. The minimum temperature for the synthesis of pure NPD, below which a small amount of compressed graphite was formed, significantly increased with pressure from ～1700°C at 15?GPa to ～1900°C at 25?GPa. The NPD having grain sizes less than ～50?nm was synthesized at temperatures below ～2000°C at 15?GPa and ～2300°C at 25?GPa, above which significant grain growth was observed. The grain size of NPD decreases with increasing pressure and decreasing temperature, and the pure NPD with grain sizes less than 10?nm is obtained in a limited temperature range around 1800–2000°C, depending on pressure. The pure NPD from glassy carbon is highly transparent and exhibits a granular nano-texture, whose grain size is tunable by selecting adequate pressure and temperature conditions.     

Effect of thermomechanical processing on microstructural evolution and deformation behaviour of polycrystalline magnesium under quasi-static and high strain rate conditions

Abstract

The effect of thermomechanical processing on microstructure evolution and room temperature flow behaviour of polycrystalline magnesium in compression at strain rates of ~10^?2 and ~10³ s^?1 was investigated. Different initial microstructures were produced by optimising rolling and annealing cycles. Prior to annealing for 1 h at 350 °C, Mg samples were processed by two different treatments such as (i) hot rolling at 350 °C and (ii) hot rolling at 350 °C plus cold rolling at room temperature. Introduction of cold working step led to an increased fraction of hard oriented grains with a marginal grain size difference in post-annealed samples. A profound effect of thermomechanical processing on strain hardening rate as well as rate-sensitive flow behaviour of Mg was observed. The influence of prior processing history and strain rate on flow behaviour of Mg was clearly reflected in terms of texture strengthening/weakening phenomena and formation of microstructural deformation bands.     

Crystallization behaviour of PZT in multilayer heterostructures

Microstructural and electrical properties of PZT (lead zirconate titanate) thin films prepared by sol-gel techniques at annealing temperatures in the range from 550°C to 900°C are studied. Perovskite (Pe) grain nucleation in PZT film starts but not completes at 550°C. Along with formation of round Pe (111) grains on the Pt (111) interface, the film contains small Pe and pyrochlore (Py) grains. Films annealed at the temperatures higher than 600°C demonstrate column structure of Pe grains, the amount of Py inclusions reduces with the annealing temperature and practically disappears at 700°C. An increase of annealing temperature leads to enhancement of (100) Pe orientation as a result of Ti diffusion on the Pt surface. Polarization decreases with the annealing temperature (maximum at 600°C), whereas permittivity increases up to the annealing temperature of 750°C.     

Austenite grain growth kinetics and mechanism of grain growth in 12Cr ultra-super-critical rotor steel

ABSTRACT

In this paper, the austenite grain growth behaviour of 12Cr ultra-super-critical (USC) rotor steel was investigated by a series of heat treatments. The heat treatments at heating temperatures of 900°C–1250°C and holding time of 1?h–20?h were conducted in an electric box-type heating furnace. Experimental results showed that the sizes of austenite grain were affected by heating temperatures and holding time, and heating temperature was the dominant factor. In addition, the grain growth rate changed significantly before and after the turning points of 1050°C and 1250°C. Meanwhile, an austenite grain growth mathematical model was established at different heating temperature stages, and possession of the capability to accurately predict austenite grain size was confirmed. Furthermore, the microstructure of austenite grain in the heating process was observed by optical microscope (OM) and transmission electron microscopy (TEM), which revealed the mechanism of austenite grain growth. Analysis indicated that the change of quantity of precipitate particles with increasing heating temperature was the main reason for the difference in austenite grain growth.     

Mechanism of texture and microstructure evolution during warm rolling of Ti–6Al–4V alloy

Ti–6Al–4V (Ti64) plates were subjected to rolling at 600°C and 800°C, respectively, for reductions up to 90% reduction in thickness. The mechanism of texture and microstructure evolution during rolling was studied in the present study. Extension twins of coherent nature were observed in the samples rolled up to 50% of reduction. The deformation was relatively inhomogeneous in the samples rolled at 600°C compared to that at 800°C. Visco-plastic self-consistent (VPSC) simulation showed that relative activity of pyramidal <c+a> slip was higher during rolling at 800°C compared to that at 600°C. The average activity of slip systems per grain was less than five for the samples rolled at 600°C and this might be responsible for the strain heterogeneity in the large grains. Further, twinning activity was found to be limited to a true strain of 0.5, as supported by the microstructural observation. VPSC simulation also showed the presence of contraction twins in the samples which was further supported by X-ray texture measurement. Dominant basal texture was observed in the samples irrespective of the temperature of rolling.     

Deformation and annealing behaviour of a low carbon high Mn TWIP steel microalloyed with Ti

ABSTRACT

A low carbon high Mn, Ti microalloyed dual phase TWIP steel has been processed through cold rolling and annealing. X-ray diffraction reveals the maximum austenite (≈92%) in HRACST sample whereas, the 50CD sample shows 29% ferrite. The microstructure of HRAC and HRACST samples reveal austenite grains with annealing twins and deformation induced ferrite (DIF). The higher amount of DIF along with deformation twins form during cold deformation. Annealing at 500°C shows recovery, whereas at 700°C shows partial recrystallisation and at 900°C reveals almost full recrystallisation. TEM microstructures of the 900°C for 30?min samples reveal annealing twins with TiC particle. Strong Brass {110}<112> and Goss{110}<001> texture components are observed in HRAC, HRACST and 50CD samples. Goss Twin (GT) {113}<332> and Copper Twin (Cu-T) {552}<115> components are observed in 50CD sample. Addition of Ti results in an average grain size of 20?μm. Maximum YS (1176?MPa) and UTS (1283?MPa) values with the lowest ductility of 11% have been obtained for the 50CD sample which is related to the formation of extensive deformation twin and a higher fraction of DIF. 700°C-30?min and 700°C-60?min samples show an increase in ductility (23% and 34%, respectively) with a marginal decrease in tensile strength (1054?MPa). Annealing at 900°C shows ductility restoration up to 60% with higher tensile strength compared to HRACST sample. Ductile fracture of HRAC and HRACST samples transform to brittle fracture in the 50CD sample. Annealing at 900°C for 30?min shows ductile fracture with some (Fe, Mn)S and TiC particles.     

Modelling of austenite grain growth kinetics in a microalloyed steel (30MSV6) in the presence of carbonitride precipitates

Austenite grain growth kinetics in the presence of secondary precipitates of a microalloyed steel (30MSV6) was studied employing quantitative metallographic techniques. Austenitizing experiments were carried out at 1,000, 1,100 and 1,200?°C. According to the experimental data, abnormal grain growth behaviour is observed at 1,100?°C while it is normal at 1,000 and 1,200?°C. TEM observation represents multicomponent carbonitride precipitate, (Ti,V)(C,N), in the as-received steel with a mean radius of 35?nm. A mathematical model is proposed considering austenite grain growth along with dissolution and coarsening kinetics of the multicomponent precipitates. The austenite grain growth model for short-term non-isothermal and subsequent long-term isothermal heating stages was developed using a statistical approach. The model includes an algorithm to estimate the size distribution of austenite grains. Precipitate mean field dissolution and Lifshitz–Slyozov–Wagner coarsening models were integrated in the proposed model to calculate the pinning pressure retarding the grain boundary movement. The mean austenite grain size and the grain size distribution (normal and abnormal) calculated by the model are in good agreement with experimental data.     

Influence of composition on hyperfine interactions in FeMoCuB nanocrystalline alloy

Influence of varying Fe/B ratio upon hyperfine interactions is investigated in the Fe_91?x Mo₈Cu₁B_x rapidly quenched alloys. They are studied both in the as-quenched (amorphous) state as well as after one-hour annealing at different temperatures ranging from 330 °C up to 650 °C. Such a heat treatment causes significant structural changes featuring a formation of nanocrystalline bcc-Fe grains during the first crystallization step. At higher annealing temperatures, a grain growth of bcc-Fe and occurrence of additional crystalline phases are observed. The relative fraction of the crystalline phase governs the development of magnetic hyperfine fields in the residual amorphous matrix even if this was fully paramagnetic in the as-quenched state. The development of hyperfine interactions is discussed as a function of annealing temperature and composition of the investigated alloys. ⁵⁷Fe Mössbauer spectrometry was used as a principal analytical method. Additional information related to the structural arrangement is obtained from X-ray diffractometry. It is shown that in the as-quenched state, the relative fraction of magnetic hyperfine interactions increases as the amount of B rises. In partially crystalline samples, the contribution of magnetic hyperfine interactions inside the retained amorphous matrix increases with annealing temperature even though the relative fraction of amorphous magnetic regions decreases.     

Abnormal grain growth in Ni-5at.%W

The growth of abnormally large grains in textured Ni-5at.%W substrates for high-temperature superconductors deteriorates the sharp texture of these materials and thus has to be avoided. Therefore the growth of abnormal grains is investigated and how it is influenced by the grain orientation and the annealing atmosphere. Texture measurements and grain growth simulations show that the grain orientation only matters so far that a high-angle grain boundary exists between an abnormally growing grain and the Cube-orientated matrix grains. The annealing atmosphere has a large influence on abnormal grain growth which is attributed to the differences in oxygen partial pressure.     

The influence of substrate temperature on the morphology, optical and electrical properties of thermal-evaporated ZnTe Thin Films

The structural, morphological, optical and electrical properties of ZnTe films deposited by evaporation were investigated as a function of substrate temperature (at −123 and 27 °C) and post-deposition annealing temperature (at 200, 300 and 400 °C). It was determined that films deposited at both substrate temperatures were polycrystalline in nature with zinc-blende structure and a strong (1 1 1) texture. A small Te peak was detected in XRD spectra for both substrate temperatures, indicating that as-deposited ZnTe films were slightly rich in Te. Larger grains and a tighter grain size distribution were obtained with increased substrate temperature. Scanning electron microscopy (SEM) studies showed that the microstructures of the as-deposited films agreed well with the expectations from structure zone model. Post-deposition annealing induced further grain growth and tightened the grain size distribution. Annealing at 400 °C resulted in randomization in the texture of films deposited at both substrate temperatures. Optical spectroscopy results of the films indicated that the optical band gap value increased from 2.13 to 2.16 eV with increased substrate temperature. Increasing the annealing temperature sharpened the band-edge. Resistivity measurements showed that the resistivity of films deposited at substrate temperatures of −123 and 27 °C were 32 Ω cm, and 1.0 × 10⁴ Ω cm, respectively with corresponding carrier concentrations of 8.9 × 10¹⁵ cm⁻³ and 1.5 × 10¹⁴ cm⁻³. Annealing caused opposite changes in the film resistivity between the samples prepared at substrate temperatures of −123 and 27 °C.     

Grain evolution of nano-crystals ZnO under HP and HT

Grain evolution of nano-crystals ZnO under high temperature and pressure is studied using a cubic high pressure apparatus. The structure, grain sizes and morphology of the samples are characterized by X-ray diffraction and field emission scanning electron microscopy. The results show that the grain sizes of ZnO grow rapidly at temperature 200°C under pressure. At temperature lower than 300°C (including 300°C), the grain sizes of the samples first increase with the pressure increasing from 1 to 3 GPa and later decrease from 4 to 6 GPa. The activation volume from 1 to 3 GPa and from 4 to 6 GPa is calculated respectively using the phenomenological kinetic grain growth equation at temperature 300°C. At temperature higher than 400°C (including 400°C), the grain sizes of the samples increase with the pressure increasing from 1 to 6 GPa. ZnO nano-bulks with good quality can be obtained under the specific conditions.     

Temperature dependent surface and spectral modifications of nano V<Subscript>2</Subscript>O<Subscript>5</Subscript> films

Nanocrystalline V₂O₅ films have been deposited on glass substrates at 300°C substrate temperature using thermal evaporation technique and were subjected to thermal annealing at different temperatures 350, 400, and 550°C. X-ray diffraction (XRD) spectra exhibit sharper and broader characteristic peaks respectively indicating the rearrangement of nanocrystallite phases with annealing temperatures. Other phases of vanadium oxides started emerging with the rise in annealing temperature and the sample converted completely to VO₂ (B) phase at 550°C annealing. FESEM images showed an increase in crystallite size with 350 and 400°C annealing temperatures followed by a decrease in crystallite size for the sample annealed at 550°C. Transmission spectra showed an initial redshift of the fundamental band edge with 350 and 400°C while a blue shift for the sample annealed at 550°C, which was in agreement with XRD and SEM results. The films exhibited smart window properties as well as nanorod growth at specific annealing temperatures. Apart from showing the PL and defect related peaks, PL studies also supported the observations made in the transmission spectra.     

The influence of Si on the microstructure and sintering behavior of ultrafine WC

The microstructure of sintered nanoscale tungsten carbide powders with 1?wt % Si addition was found to be populated by an abnormally large number of elongated grains. Interrupted sintering experiments were conducted to clarify the origins of the excessive abnormal grain growth seen in the microstructure. It was observed that rapid coarsening occurred at high temperatures owing to the formation of a liquid phase. However, the grain shape evolution during this coarsening period was found to be a consequence of excessive stacking faults and micro twins on the basal planes probably generated by reaction of WC with Si. Analyses of the microstructures and the isothermal and non isothermal coarsening behaviors suggested that the platelet morphology evolved by defect-assisted nucleation and growth on faceted grains. Based on experimental evidence from samples interrupted at low temperatures and crystal growth theories, we discuss the possible mechanisms that eventually led to the rampant platelet-type morphology. Further, the influence of such rapid grain growth on the shrinkage rate during sintering is also discussed. In comparison with the cyclic coarsening-densification process of sintering in pure nanoscale WC, the addition of Si leads to only two distinct sintering stages: either densification dominated or coarsening dominated. Concurrent densification and coarsening cannot be sustained particularly in the presence of a liquid phase that significantly enhances coarsening.     

Influence of precipitate-assisted nucleation on the microstructure and mechanical properties of Al-Mg-Si-Cu-Zn alloys

The influence of precipitation on the recrystallization nucleation and mechanical properties of Al-Mg-Si-Cu-Zn alloys was investigated by means of tensile tests, SEM, TEM, XRD and EBSD. The results reveal that there are distinct contributions from the various precipitates that form during annealing and that these critically influence the evolution of microstructure and its associated texture, as well as mechanical behaviour. In contrast to alloy sheets A, B, and C annealed at a lower temperature or for a shorter time, the T4P alloy sheet D with an annealing at 450°C for 3?h not only possesses almost identical strength and elongation, but also a higher average r (0.659) and n (0.313) values, and also a lower Δr (0.091) value. After solution treatment, the four alloy sheets are comprised of equiaxed grains with somewhat different grain sizes and different textures, but texture volume fraction and grain size in alloy sheet D both are decreased due to the effect of precipitate-assisted nucleation during solution treatment. The corresponding nucleation and growth mechanisms of recrystallization grains were established and the relationship between textures and r value in the four alloy sheets was also analyzed on the basis of a Visco-plastic self-consistent (VPSC) model.     

Fabrication and Characterization of CuO nanowires on V-shaped Microgroove surfaces

This study developed a facile and scalable thermal oxidation method to prepare CuO nanowires on the electro-discharge machining (EDM) processed V-shaped microgrooves. The formation feasibility, surface morphology, and wetting properties of nanowires on V-shaped microgrooves were explored by the variation of thermal oxidation temperatures from 300 to 600 °C, and oxidation times from 2 h to 8 h. Nanowires were found to successfully synthesized on the V-shaped microgrooves surfaces when annealing temperature was 400 °C or higher. The microvoids or microcavities on the EDM processed V-shaped microgrooves surfaces contributed to the stress grain boundary (GB) diffusion of copper atoms, and facilitated the growth of nanowires. The diameter of nanowires increased monotonically when the annealing temperatures increased, whereas it almost kept unchanged with increasing annealing times. The length of nanowires was influenced positively by both annealing temperature and annealing time. All the nanowire samples showed hydrophobic properties of water.