Orientation dependence of the substructure characteristics in a Ni-30Fe austenitic model alloy deformed in hot plane strain compression

The present work examines in detail the substructure and texture characteristics in a Ni-30Fe austenitic model alloy subjected to deformation by plane strain compression (PSC) at temperatures between 700 and 900 °C to strains between 0.2 and 1 using a strain rate of 1 s⁻¹. The flow curves display characteristics typical of limited dynamic recrystallization. The deformed matrix texture is similar to that expected for rolling/PSC deformation of face-centred cubic metals while the comparatively weaker dynamic recrystallization texture is dominated by the Cube component. The non-Cube deformed matrix grains contain “organized”, self-screening arrays of microbands aligned along the slip planes with high Schmid factors. By contrast, the Cube deformed matrix grains exhibit more “random” cell substructure with a low density of superimposed larger-angle dislocation walls. These walls are related to {1 1 1} slip planes at low strains, but tend to follow the rigid body rotation toward the compression plane at large strains.     

A thermodynamic approach on vapor-condensation of corrosive salts from flue gas on boiler tubes in waste incinerators

Thermodynamic equilibrium calculation was conducted to understand the effects of tube wall temperature, flue gas temperature, and waste chemistry on the type and amount of vapor-condensed “corrosive” salts from flue gas on superheater and waterwall tubes in waste incinerators. The amount of vapor-condensed compounds from flue gases at 650-950 °C on tube walls at 350-850 °C was calculated, upon combustion of 100 g waste with 1.6 stoichiometry (in terms of the air-fuel ratio). Flue gas temperature, rather than tube wall temperature, influenced the deposit chemistry of boiler tubes significantly. Chlorine, sulfur, sodium, potassium, and calcium contents in waste affected it as well.     

Solution-phase chemical route to branched single-crystalline CdS nanoarchitectures and their field emission property

A facile solution chemical method is developed to prepare hierarchical branched single-crystalline CdS architectures. A mechanism of “nucleate-aggregate-grow-ripen-separate” process is proposed to illustrate the growth of the CdS architectures. The obtained branched CdS architectures exhibit superior FE properties with the lower turn-on field (Eto) of 7.1 V μm⁻¹ at a current density of 10 μA cm⁻², and threshold field (Ethr) of 8.3 V μm⁻¹ at a current density of 100 μA cm⁻², which shows that the obtained products have greatly potential application as FE devices.     

Dislocation starvation and exhaustion hardening in Mo alloy nanofibers

The evolution of defects in Mo alloy nanofibers with initial dislocation densities ranging from 0 to ∼1.6 × 10¹⁴ m⁻² were studied using an in situ “push-to-pull” device in conjunction with a nanoindenter in a transmission electron microscope. Digital image correlation was used to determine stress and strain in local areas of deformation. When they had no initial dislocations the Mo alloy nanofibers suffered sudden catastrophic elongation following elastic deformation to ultrahigh stresses. At the other extreme fibers with a high dislocation density underwent sustained homogeneous deformation after yielding at much lower stresses. Between these two extremes nanofibers with intermediate dislocation densities demonstrated a clear exhaustion hardening behavior, where the progressive exhaustion of dislocations and dislocation sources increases the stress required to drive plasticity. This is consistent with the idea that mechanical size effects (“smaller is stronger”) are due to the fact that nanostructures usually have fewer defects that can operate at lower stresses. By monitoring the evolution of stress locally we find that exhaustion hardening causes the stress in the nanofibers to surpass the critical stress predicted for self-multiplication, supporting a plasticity mechanism that has been hypothesized to account for the rapid strain softening observed in nanoscale bcc materials at high stresses.     

Phase transformations in low-temperature chromized 0.45 wt.% C plain carbon steel

The phase transformations occurring in a 0.45 wt.% C plain steel subjected to plasma nitriding at 540-560 °C for 5.5 h, followed by a salt bath thermoreactive deposition and diffusion (TRD) chromizing process at 500 °C or 550 °C (a process referred to as low-temperature chromizing or duplex chromizing) was investigated by means of optical microscopy(OM), scanning electron microscopy(SEM), X-ray energy dispersive spectroscopy(EDS), and X-ray diffraction. It was found that a CrN compound layer with an average thickness of 7.4 μm and an average micro-hardness of 1476 HV_0.01 was formed in the prior plasma nitrided compound layer by low-temperature chromizing at 550 °C for 6 h. The chromized coating as a whole was found consisting of three sub-layers, namely the outer CrN layer, the intermediate diffusional layer, and the inner residual nitrided compound layer, all formed in the prior nitrided compound layer, and with the inner sub-layer vanishing by prolonging the chromizing time. The intermediate diffusional layer formed at the initial stages of TRD was seen “black” under OM (hence is called “black zone”), and found consisting of α-Fe as a major phase. The self-exhaustion of the “black zone” promoted the chromium atom diffusion deeper into the substrates. The transformation paths involved in the decomposition of the prior nitrided compound layer was likely to be ε-Fe_2-3N → γ′-Fe₄N → α-Fe; and the high hardness of the chromized coating was attributed to a large amount of nano-sized and evenly distributed CrN grains generated in the compound layer.     

High thermal stability of TiAlSiCN coatings with “comb” like nanocomposite structure

The aim of this work was to understand the reasons for the exceptionally high thermal stability of the TiAlSiCN coatings. The hardness of the coatings increased from 41.5 to 43 GPa between 25 and 900 °C, reached a maximum value of 49 GPa at 1000 °C, and then decreased to 37 GPa at 1300 °C. The structural investigations performed before and after annealing at 1000, 1200, and 1400 °C using X-ray diffraction, scanning and transmission electron microscopy (TEM), and high-resolution TEM showed that the as-deposited “comb” like nanocomposite structure, in which (Ti,Al)(C,N) columnar grains, 10–30 nm wide, were separated by a well developed amorphous tissue, possessed a very high thermal stability as its dominant cubic phase was stable in the temperature range of 25–1400 °C. Further thorough characterization by means of energy-dispersive spectroscopy, X-ray photoelectron spectroscopy, and Raman spectroscopy revealed structural modifications inside crystalline and amorphous phases during annealing in vacuum. Such modifications associated with a short-range rearrangement of elements are shown to be responsible for the high hardness of the TiAlSiCN coatings observed up to 1300 °C, with peak hardness at 1000 °C.     

Kinetics and driving forces of abnormal grain growth in thin Cu films

The abnormal growth of individual (1 0 0) oriented grains is monitored by the in situ electron backscatter diffraction technique for more than 24 h at three different annealing temperatures (90 °C, 104 °C and 118 °C) in 1-5 μm thick Cu films on polyimide substrates. The (1 0 0) grain growth velocity increases with higher film thickness and annealing temperature, as suggested by an earlier model by Thompson and Carel. As a result, the final (1 0 0) texture fraction becomes more dominant for higher annealing temperatures and larger film thicknesses. The Thompson-Carel model, however, predicts that the (1 1 1) grains will preferably grow at temperatures up to 118 °C. Our calculations of the driving forces revealed that in addition to minimization of the strain energy (due to the thermal mismatch between film and substrate) and of the surface energy, the energy stored in the dislocations plays a decisive role in grain growth. Our observations can be understood by the notion that initially available (1 0 0) grain nuclei start to grow very rapidly, due to dislocation annihilation, and thus “overrun” the (1 1 1) grains in size.     

Microstructure characterization of as-fabricated and 475 °C annealed U-7 wt.% Mo dispersion fuel in Al-Si alloy matrix

High-density uranium (U) alloys with an increased concentration of U are being examined for the development of research and test reactors with low enriched metallic fuels. The U-Mo fuel alloy dispersed in Al-Si alloy has attracted particular interest for this application. This paper reports our detailed characterization results of as-fabricated and annealed (475 °C for 4 h) U-Mo dispersion fuels in Al-Si matrix with a Si concentration of 2 and 5 wt.%, named as “As2Si”, “As5Si”, “An2Si”, “An5Si” accordingly. Techniques employed for the characterization include scanning electron microscopy and transmission electron microscopy with specimen prepared by focused ion beam in situ lift-out. Fuel plates with Al-5 wt.% Si matrix consistently yielded thicker interaction layers developed between U-Mo particles and Al-Si matrix, than those with Al-2 wt.% Si matrix, given the same processing parameters. A single layer of interaction zone was observed in as-fabricated samples (i.e., “As2Si”, “As5Si”), and this layer mainly consisted of U₃Si₃Al₂ phase. The annealed samples contained a two-layered interaction zone, with a Si-rich layer near the U-Mo side, and an Al-rich layer near the Al-Si matrix side. The U₃Si₅ appeared as the main phase in the Si-rich layer in “An2Si” sample, while both U₃Si₅ and U₃Si₃Al₂ were identified in sample “An5Si”. The Al-rich layer in sample “An2Si” was amorphous, whereas that in sample “An5Si” mostly consisted of crystalline U(Al,Si)₃, along with a small fraction of U(Al,Si)₄ and U₆Mo₄Al₄₃ phases. The influence of Si on the diffusion and reaction in the development of interaction layers in U(Mo)/Al(Si) is discussed in the light of growth-controlling mechanisms and irradiation performance.     

Electromagnetic reduction of a pre-formed radius on AA 5754 sheet

Electromagnetic (EM) forming is a high-speed forming process that uses the forces induced on a conductive workpiece by a transient high frequency current to form the workpiece into a desired shape. This paper presents the results of an experimental and numerical study carried out to determine whether EM forming techniques could be used to obtain sharper radii in aluminum alloy AA 5754 compared to that attained using conventional stamping process alone. AA 5754 1 mm sheet was formed into a v-shape with a 20 mm outer radius and then the radius was reduced or “sharpened” to 5 mm using EM forming. This “hybrid” process was modeled numerically to gain insight into the process and the challenges involved in the numerical simulation of the physical phenomena that are present in this process. As with any novel process, there are limitations and issues that must be addressed if this technique is to be implemented commercially; however; the research indicates that features that are not achievable using traditional stamping techniques can be obtained using EM forming.     

Carbon tetrafluoride plasma modification of polyimide: A method of in-situ formed hydrophilic and hydrophobic surfaces

This study demonstrates that carbon tetrafluoride (CF₄) plasma can result in relatively hydrophobic and hydrophilic surfaces formed in-situ on polyimide (PI) films using a mask and controlling the distance of the mask to the substrate. The surface properties of plasma-treated PI films are characterized by contact angle measurement, atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). Under specific modification conditions, contact angles for hydrophobic and hydrophilic surfaces reach values of 108.3 ± 0.6° and below 5°, respectively. The XPS analyses indicate that the “unshielded” surfaces contained a high proportion of the CF₂-CF₂ group and therefore decreased the wettability of the surface. On the other hand, the “shielded” surface contained hydrophilic groups such as carbonyl or carboxyl with few fluorinated groups, resulting in increased wettability of the surface.     

Reactive wetting during hot-dip galvanizing of high manganese alloyed steel

The present study discusses reactive wetting during hot-dip galvanizing of high Mn alloyed steel (X-IP1000, 23 wt.% Mn) and is focused on investigating the influence of the metallic Mn concentration in the steel bulk composition on phase formation at the interface steel/coating. Samples were in-line bright annealed (1100 °C/ 60 s in N2-5%H2 at DP −50 °C) prior hot-dipping to avoid external MnO on the steel surface. This approach was applied to avoid influencing the wetting reaction by an aluminothermic MnO reduction, because this is considered to lead to an unwanted zeta-phase (FeZn13) formation in the coating by hot-dipping of Mn alloyed steels (< 5.0 wt.% Mn). The influence of hot-dipping parameters, which are contributing to the kinetics of the wetting reaction, was examined in terms of varying bath-Al content (0.17 and 0.22 wt.%), bath temperature (440-500 °C) and strip entry temperature (420-520 °C). The structure and chemical composition of both galvanized coating and interface steel/coating were characterized. While external MnO was verifiably avoided, brittle zeta-phase distinctively appeared at the interface steel coating together with the typical Fe₂Al₅ phase. This shows that the model of aluminothermic MnO reduction failed in the present case. This study suggests an alternative model explaining the appearance of zeta-phase with the removal of bath-Al by metallic Mn, which is dissolved out of the steel bulk into the Zn bath. The present investigation shows that alloying elements in the steel bulk may influence coating quality not only “indirectly” by external formation of nonwettable oxides, but also “directly” by influencing phase equilibria and kinetics of the wetting reaction. Understanding these phenomena will improve processing of (high) alloyed steel concepts as well as industrial Zn bath management.     

Cyclic oxidation behavior and thermal barrier effect of YSZ-(Al2O3/YAG) double-layer TBCs prepared by the composite sol-gel method

Novel YSZ (6 wt.% yttria partially stabilized zirconia)-(Al₂O₃/YAG) (alumina-yttrium aluminum garnet, Y₃Al₅O₁₂) double-layer ceramic coatings were fabricated using the composite sol-gel and pressure filtration microwave sintering (PFMS) technologies. The thin Al₂O₃/YAG layer had good adherence with substrate and thick YSZ top layer, which presented the structure of micro-sized YAG particles embedded in nano-sized α-Al₂O₃ film. Cyclic oxidation tests at 1000 °C indicated that they possessed superior properties to resist oxidation of alloy and improve the spallation resistance. The thermal insulation capability tests at 1000 °C and 1100 °C indicate that the 250 μm coating had better thermal barrier effect than that of the 150 μm coating at different cooling gas rates. These beneficial effects should be mainly attributed to that, the oxidation rate of thermal grown oxides (TGO) scale is decreased by the “sealing effect” of α-Al₂O₃, the “reactive element effect”, and the reduced thermal stresses by means of nano/micro composite structure. This double-layer coating can be considered as a promising TBC.     

In situ micro-cantilever tests to study fracture properties of NiAl single crystals

In situ micro-cantilever tests were carried out to determine the anisotropic fracture toughness of NiAl single crystals. Notched micro-cantilever beams with a beam length of 8 μm, 1.5 μm thickness and 1.8 μm width were milled in so-called “hard” and “soft” orientations of NiAl using a focused ion beam. These cantilevers were loaded in situ with the help of a cantilever-based nanoindenter mounted inside a scanning electron microscope. A fracture toughness of 3.52 ± 0.29 MPa m^1/2 was obtained for the “soft” orientation and 5.12 ± 0.50 MPa m^1/2 for the “hard” orientation, which is in good agreement with literature values on the fracture toughness of macroscopic NiAl specimens. Furthermore, nanoindentations were performed for studying the size effects occurring at small length scales for both orientations. The applicability of the small sample geometries for testing the fracture toughness is finally discussed in terms of size effects in the flow stress of the material due to dislocation nucleation and strain gradients at the crack tip.     

Plate forging of tailored blanks having local thickening for deep drawing of square cups

A plate forging process of tailored blanks having local thickening for the deep drawing of square cups was developed to improve the drawability. A sheet having uniform thickness was bent into a hat shape of two inclined portions, and then was compressed with a flat die under restraint of both edges to thicken the two inclined portions. The bending and compression were repeated after a right-angled rotation of the sheet for thickening in the perpendicular direction. The thickness of the rectangular ring portion equivalent to the bottom corner of the square cup was increased, particularly the thickening at the four corners of the rectangular ring undergoing large decrease in wall thickness in the deep drawing of square cups became double. The degree of thickening can be adjusted by controlling the punch stroke in the bending. By using the tailor blanks having local thickening, not only the decrease in wall thickness at the bottom corner of the square cup was prevented, but also the limiting drawing height of the cup without fracture was increased to 28.3 mm, whereas that for the uniform blank was 21.3 mm.     

Depth profiling of defects in ion-implanted Ni and Fe by positron annihilation measurements

Pure Ni and Fe samples were irradiated with 150 keV Ar ions at room temperature, 300 and 500 °C to introduce defects near the surface. The irradiated samples were characterized by energy-variable slow-positron beams with Doppler broadening and positron lifetime measurements to investigate defect profiles. The irradiation-induced defects were detected at regions much deeper than ion projected ranges for all the temperatures. The origin of such defects beyond the projected ranges was discussed in terms of vacancy migration, ion channeling, surface contamination and depth-scale error. Among these effects, the ion channeling may account for the obtained results.     

Effect of β grain growth on variant selection and texture memory effect during α → β → α phase transformation in Ti-6 Al-4 V

In the present study, the texture evolution and the role of β grain growth on variant selection during β → α phase transformation have been investigated in Ti-6 Al-4 V with and without 0.4 wt.% yttrium addition. The aim of adding yttrium was to control β grain growth above the β transus by pinning grain boundaries with yttria. Both materials were first thermomechanically processed to generate similar starting microstructures and crystallographic textures. Subsequently, both materials were solution-heat-treated above the β transus followed by slow cooling to promote growth of the α lath structure from grain boundary α. Additional interrupted slow cooling experiments were carried out to identify the α lamellae that nucleate first from β grain boundaries. Detailed electron backscatter diffraction analysis was carried out and it was found that the β heat treatment did not generate new texture components although the intensities of the individual components changed dramatically depending on the alloy/β grain size. Variant selection was assessed by comparing measured α texture components with predicted α texture components based on the high-temperature β texture assuming equal variant selection. It was found that with increasing β grain size variant selection intensified favouring the {φ1, Φ, φ2} {90°, 30°, 0°} texture component. Interrupted cooling experiments revealed that α nucleates first on β grain boundaries that are formed by two β grains having a common (1 1 0) normal and that these α lamellae display almost exclusively a {φ1, Φ, φ2} {90°, 30°, 0°} orientation. Consequently, the dominance of this variant with increasing β grain size can be related to the relative free growth of this particular α texture component into an “empty” β grain.     

On the influence of small quantities of Bi and Sb on the evolution of microstructure during swaging and heat treatments in copper

In the present work, the influence of small amounts of Bi and Sb on the microstructural evolution of Cu during an ingot metallurgy processing route is investigated. Both elements are known to segregate to grain boundaries in Cu. Cu ingots with an outer diameter of 40 mm containing 0.008 wt.% Bi and 0.92 wt.% Sb, respectively, were vacuum induction melted, cast, and gradually swaged down to a final diameter of 11.7 mm with several intermediate annealing steps. Subsequent annealing treatments were conducted to investigate the microstructural evolution of the swaged bars. Optical microscopy, hardness testing and orientation imaging microscopy were used to characterize the deformation and recrystallization behavior, as well as the evolution of texture in the alloys. The results are then compared to those obtained for pure Cu. It is shown that even small amounts of alloying elements significantly alter the hardening behavior and suppress recrystallization at low temperatures. At higher temperatures, recrystallization in Cu, Cu-Bi and Cu-Sb leads to different textures.     

Sinter and hot isostatic pressing (HIP) of multi-wall carbon nanotubes (MWCNTs) reinforced ZTA nanocomposite: Microstructure and fracture toughness

This work describes the microstructure and fracture toughness of zirconia toughened alumina (ZTA) nanocomposite in which multi-wall carbon nanotubes (MWCNTs) and nanosized ZrO₂ particles were used as reinforcement. The ZTA nanocomposites with additions of 0, 0.005, and 0.01 wt.% MWCNTs and 2 wt.% nanosized ZrO₂ particles were pressureless sintered in an anti-oxidant sagger with graphite powder bed at 1520 °C during 1 h in air and then HIPed at 1475 °C in argon atmosphere 1 h at a pressure of 150 MPa. Relative densities ranging 94–98% were reached. In HIPed composites the hardness and fracture toughness values were increased up to ∼17% and ∼37%, respectively, compared to the “as sintered” composites free of carbon nanotubes. A combined fracture mode, crack deflection, pull-outs of a small amount of carbon nanotubes, and bridging effect were the mechanisms leading to the improvement in fracture toughness.     

The effect of partially cut-out blanks on geometric accuracy in incremental sheet forming

Industrial requirements for accuracy in metal sheet components are typically ±0.2 mm where current incremental sheet forming processes are capable of an accuracy of only ±3 mm. Several approaches based on process design modifications or control strategies are being developed to overcome this problem, but none has as yet been entirely successful. This paper proposes and examines a new approach in which the area to be formed within the blank is “partially cut-out” using a water jet or laser cutter. The aim of this partial cut-out is to localise deformation to the area over which the tool travels and thus reduce the difference between a part made by a “contour tool path” and the target product geometry. Several design options are considered, and the approach is evaluated with one simple and one complex part. The results indicate that partially cut-out blanks lead to slightly more accurate forming than conventional blanks when unsupported, but that the accuracy improvement is less than that which is achieved by use of a stiff cut-out supporting plate. The results include an experimental investigation of residual stresses and springback in incremental sheet forming.     

Figure of merit for the quality of ZrO2 coatings on stainless steel and nickel-based alloy surfaces

A figure of merit (FOM) has been developed to define the quality of ceramic (e.g., ZrO₂) coatings on metal and alloy [Type 304SS and Alloy 600] surfaces. Zirconia (ZrO₂) coatings were developed as a means of protecting the metal/alloy surfaces from stress corrosion cracking (SCC) in boiling water reactor (BWR) primary heat transport circuits, by inhibiting the cathodic reaction (reduction of oxygen and hydrogen peroxide) on the surface external to the crack. The distribution of pores in the coating plays an important role in corrosion prevention, such that the lower the porosity of the coating, the better the protection afforded to the system against SCC. Since the reactors operate at high temperature (e.g., at 288 °C under full power conditions), the temperature dependence of the FOM was investigated. The figure of merit (FOM) was developed by measuring impedance data over a wide range of frequency (10 mHz-5 kHz) at temperatures of 25, 100, 200, and 288 °C in hydrogenated, buffered solutions, with the hydrogen electrode reaction (HER) being used as a “fast” redox couple. An “equivalent circuit” analog was first developed from the bare surface impedance data and this analog was then employed in a second step to model the pore bottom in defining the pore distribution on the coated surface. A lognormal distribution (LND) of the pores was assumed and the parameters of the LND were determined using a constrained optimization technique to fit the model to the experimental data for the coated surface at different temperatures. The results suggest that, as temperature increases, the coating becomes more porous, making the substrate more susceptible to corrosion cracking. At 288 °C, 87% of the SS and 85% of the Ni-alloy surfaces become porous with the pore radius varying from 0.0001 cm to 0.01 cm.