Dislocation structures in single-crystal tungsten and tungsten alloys

Deformation of tungsten single crystals as a function of strain, temperature, and alloying was studied by transmission electron microscopy. Single crystals oriented for (?101)[lll] slip were grown by electron beam zone refining. Compression specimens of tungsten, W-l and 3 pct Re and W-l and 3 pct Ta were deformed to 2 pct strain at 150°, 300°, and 590°K (0.04, 0.08, and 0.16T _m). Specimens were also strained to 0.5 and 5.0 pct strain at 300°K. Transmission microscopy revealed that the dislocation substructures in single-crystal tungsten are similar to substructures in other refractory metals when compared on a homologous temperature basis. At temperatures greater than 0.1T _m, the substructure is characterized primarily by edge dipoles. At temperatures less than 0.1T _m, long screw dislocations lying parallel to the primary [111] slip direction characterize the substructure. Rhenium additions to tungsten promote formation of edge dipoles at temperatures of 300° and 150°K and increase dislocation density at all three temperatures. In addition, dislocations consistent with (1?12)[?111] slip were observed in the W-Re single crystals after deformation at 150°K. Tantalum additions had a lesser effect on the dislocation substructure compared to rhenium additions. The W-l and 3 pct Ta alloys exhibited higher dislocation densities than unalloyed tungsten after similar strains and, at 150°K, W-3 pct Ta contained a few dislocations consistent with (1?12)[?111] slip. It is concluded that the reduction in ductile-brittle transition temperature of poly crystalline tungsten containing dilute rhenium additions, 1 to 5 pct, can be attributed to an increase in dislocation mobility at temperatures less than 0.1 T_m.     

Analysis of the Deformation Behavior in Tension and Tension-Creep of Ti-3Al-2.5V (wt pct) at 296 K and 728 K (23 °C and 455 °C) Using In Situ SEM Experiments

The deformation behavior of a Ti-3Al-2.5V (wt pct) near-α alloy was investigated during in situ deformation inside a scanning electron microscopy (SEM). Two plates with distinct textures were examined. Tensile experiments were performed at 296 K and 728 K (455 °C) (~0.4T _m), while a tensile-creep experiment was performed at 728 K (455 °C) and 180 MPa (σ/σ _ys = 0.72). The active deformation systems were identified in the α phase using electron backscattered diffraction based slip-trace analysis and SEM images of the surface. Prismatic slip deformation was the dominant slip mode observed for all the experiments in both plates, which was supported by a critical resolved shear stress (CRSS) ratio analysis. However, due to the texture of plate 1, which strongly favored the activation of prismatic slip, the percentages of prismatic slip activity for specimens from plate 1 tested at 296 K and 728 K (23 °C and 455 °C) were higher than the specimens from plate 2 under the same testing conditions. T1 twinning was an active deformation mode at both 296 K and 728 K (23 °C and 455 °C), but the extent of twinning activity decreased with increased temperature. T1 twinning was more frequently observed in specimens from plate 2, which exhibited a higher fraction of twinning systems favoring activation at both 296 K and 728 K (23 °C and 455 °C). The tension-creep experiment revealed less slip and more grain boundary sliding than in the higher strain rate tensile experiments. Using a previously demonstrated bootstrapping statistical analysis methodology, the relative CRSS ratios of prismatic, pyramidal 〈a〉, pyramidal 〈c+a〉, and T1 twinning deformation systems compared with basal slip were calculated and discussed in light of similar measurements made on CP Ti and Ti-5Al-2.5Sn (wt pct).     

Defect structures and interactions in Al-Zn eutectoid alloys

Defect structures in superplastic and nonsuperplastic Al-Zn eutectoid alloys were studied by transmission electron microscopy. Slowly cooled alloys develop a fine lamellar microstructure and are not superplastic. The equiaxed quenched and quench-aged alloys, however, are super-plastic under the proper conditions of temperature and strain rate. Quench-aging produces sub-boundaries in the aluminum-rich α phase and dislocation loops in the zinc-rich β phase. Subsequent room temperature deformation creates a typical cold-worked dislocation structure in the α phase. At higher deformation temperatures, the cold-worked structure is increasingly replaced by a recovered structure. At the same time, the dislocation loop density in the β phase decreases to lower values. During superplastic deformation at 250βC, the dislocation loops in the β phase are annihilated by interactions with glide dislocations. In the α phase, a continuous, or steady-state, dynamic recovery process appears to operate. A completely recovered structure is maintained with dislocation-free subgrains.     

Diffusion of sputtered inconel 617 coatings in titanium

INCONEL 617 coatings 10-to 13-μm thick were radio frequency (RF) magnetron sputtered onto commercially pureα-titanium substrates and heat-treated at 800 °C for 2 hours. The resulting structures were examined in cross section by scanning electron microscopy (SEM) and analytical transmission electron microscopy (TEM). Scanning electron microscopy of polished and etched cross sections showed that the coating remained continuous, and as a result of inter-diffusion, a layer66-μn thick had formed below the coating. Examination of the coating near the free surface by TEM showed it contained both M₂₃C₆ and M₆C carbide precipitates, while several micron-thick layers containing intermetallic phases such as σ,γ′, and Ti₂Ni were found near the substrate. Kirkendall voids 75 to 300 Å in diameter were present near the original INCONEL 617/α-titanium interface. The microstructure further below that interface contained a thin layer of titanium martensite and Widmanstätten α + Ti₂Ni. No TiNi or TiNi₃ was found. The diffusivity of nickel and titanium was reduced several orders of magnitude and is attributed primarily to the formation of intermetallic compounds in the coating and substrate.     

The effect of the nitrogen potential on the coarsening kinetics of VN precipitates

An Fe-1.06 pct V alloy was used to study the kinetics of coarsening of VN precipitates. Nitriding was carried out at 600 °C in purified NH₃ gas. Nitrided specimens were then annealed at 820 °C in furnace atmospheres of different NH₃/H₂ ratios. The transmission electron microscopy technique was used to measure the precipitate sizes. The data on the precipitate sizes indicate that the coarsening of the plate shaped VN precipitates seems to be diffusion controlled. The precipitate coarsening rate appears to be lowered by the increase in NH₃ content in the furnace atmosphere. The particle size distributions were found to be broader than the predictions of the LSW theory.     

Phase Relations in CaO-SiO2-Al2O3-15 mass pct CaF2 System at 1523 K (1250 °C)

CaO-SiO₂-Al₂O₃-CaF₂ is a base system of mold flux for high Al steels. Phase equilibrium in CaO-SiO₂-Al₂O₃-15 mass pct CaF₂ system at 1523 K (1250 °C) was investigated using quenching method followed by X-ray diffraction and Scanning electron microscopy equipped with energy dispersive X-ray spectroscopy. Isothermal section in this system at 1523 K (1250 °C) with Al₂O₃ being less than 25 mass pct and CaO/SiO₂ (mass pct) being between 0.43 and 1.25 was experimentally constructed. The liquidus composition and seven solid-liquid coexistence regions at 1523 K (1250 °C) were determined.     

Structure and properties of rapidly solidified dispersion-strengthened titanium alloys: Part I. Characterization of dispersoid distribution,structure, and chemistry

The feasibility of developing dispersion-strengthened powder metallurgy Ti alloys was determined in Ti-RE (RE = Ce, Dy, Er, Gd, La, Nd, or Y) alloys prepared by rapid solidification processing. The alloys were produced by electron-beam melting and splat quenching. Dispersoid precipitation and growth were studied as functions of annealing temperature, 700 to 1000 °C, for annealing times between 5 and 50,000 minutes. Dispersoid diameters, spacings, compositions, and crystal structures were characterized by transmission and scanning electron microscopy, X-ray and electron diffraction, energy-dispersive X-ray analysis, and scanning Auger microscopy. Two classes of dispersoid coarsening behavior at temperatures below theβ-transus were identified. In Ti-Ce, Ti-Gd, and Ti-Nd alloys, equilibrium rare earth sesquioxide (RE₂O₃) dispersoids form early in the annealing process and coarsen rapidly to > 1 μm diameter. The Ti-Nd alloys additionally contain large volume fractions of small (< 100 nm diameter) dispersoids. In the other Ti-RE alloys, dispersoids identified as Ti-RE-O-C compounds coarsen relatively slowly. Ti-Er is the most promising of the investigated systems for application in a multicomponent dispersion-strengthened alloy because long-time annealing at 700 to 800 °C produces stable dispersoids of 50 to 150 nm average diameter and 300 to 600 nm inter-particle spacing.     

Substructure strengthening in dispersion-strengthened nickel alloys

Pure nickel, 80 pct Ni-20 pct Cr, 98 pct Ni-2 pct ThO₂, and 78 pct Ni-20 pct Cr-2 pct ThO₂ were studied in a wide range of thermomechanical conditions to identify strengthening mechanisms in the dispersion-strengthened materials. An X-ray line profile technique was used to determine the distribution of lattice strain, the crystallite domain size and the incidence of twins and stacking faults. Transmission electron microscopy was carried out, and tensile tests were done at room temperature and at an elevated temperature. It was found that cold deformation of Ni?ThO₂ did not produce lattice strains as large as was the case with pure nickel and Ni?Cr. However, deformation of Ni?Cr?ThO₂ did generate high lattice strains, due it is thought to the influence of chromium on cross-slip. The materials containing high lattice strains recrystallized more readily on annealing or testing at high temperature. It was concluded that room temperature strength was related to domain size without regard to composition in the series investigated. Strengthening by particle-dislocation interaction was not thought to be applicable when the domain size was small compared to the interparticle spacing, or at elevated temperatures. High temperature strength was determined primarily by the presence of a polygonized dislocation substructure which was stabilized by the thoria dispersion.     

Moiré patterns in electron transmission through Au-Ni alloys

Moiré patterns were developed in the transmission electron microscopy of thinned Au-Ni alloys as a consequence of the deposition of very thin layers of gold during the thinning process. The transmission photographs showed striated patterns, and the wavelength of the striations, which were in the range 20 to 100Å, corresponded closely to the predicted Moiré spacings. The striations are not related to the true composition modulations which occur in some of these alloys as a result of the decomposition of the solid solution. The true lattice modulations are of the order 6 to 13Å. The Moiré patterns arise from gold layers which are much thinner than the alloy layer. The electron diffraction spots of the gold are thus elongated in reciprocal space in a direction normal to the surface, and this feature can greatly affect the spacing of the Moiré striations. It is shown that Moiré spacings can be useful in determining with good precision the small changes in lattice parameter which occur on the aging of the alloys, thus providing a new tool for the study of small lattice strains.     

The micro-mechanisms of tempered martensite embrittlement in 4340-type steels

A study of the micro-mechanisms of tempered martensite embrittlement was made on a series of 4340-type steels in which the contents of manganese, silicon, and trace impurities, especially phosphorus and sulfur, were varied. One plain-carbon steel was also examined. The study employed Charpy impact tests and four-point slow-bend tests coupled with an elastic-plastic stress analysis, as well as scanning electron fractography, Auger electron spectroscopy, transmission electron microscopy of extraction replicas, and magnetic measurements of the transformation of retained austenite. The results indicate that in these steels the TME phenomenon is an intergranular embrittlement problem caused by carbide precipitation on prior austenite grain boundaries which are already weakened by segregated phosphorus and sulfur. The transformation of intragranular retained austenite is concluded not to be of primary significance in the TME in these steels, although it may contribute to the magnitude of the TME toughness trough.     

The precipitation of epsilon-carbide in twinned martensite

Tempering of martensite has been investigated by means of thin foil electron microscopy in a high carbon steel, a high nickel steel, and a silicon steel. ε carbide has been unambiguously identified in each steel. It was found that the carbide was precipitated with the Jack orientation relationship: $$\begin{gathered} \left( {0001} \right)_\varepsilon \parallel \left( {011} \right)_{\alpha '} \hfill \\ \left( {10\bar 10} \right)_\varepsilon \parallel \left( {2\bar 11} \right)_{\alpha '} \hfill \\ \end{gathered} $$ In the silicon steel the ε carbide precipitated in the form of needles which grew with a \(\left[ {01\bar 10} \right]_\varepsilon \) close to \(\left[ {21\bar 1} \right]_{\alpha '} \) . This growth direction minimizes the surface energy of the needles, yet allows growth in a direction of low mismatch.     

Microstructural Evolution and Mechanical Behaviors of an Nb-16Si-22Ti-2Al-2Hf Alloy with 2 and 17 at. pct Cr Additions at Room and/or High Temperatures

X-ray diffraction analysis, scanning electron microscopy, and transmission electron microscopy were used to investigate the microstructures and orientation relationships (ORs) of Nb-16Si-22Ti-2Al-2Hf-(2,17)Cr alloys (hereafter referred to as 2Cr and 17Cr alloys, respectively). The mechanical properties of the two alloys at room and/or high temperatures were compared. The 2Cr alloy comprised Nb_SS and (α + β)-Nb₅Si₃ phases, while the 17Cr alloy consisted of Nb_SS, (α + β)-Nb₅Si₃ and Laves Cr₂Nb phases with a C15 structure. The β-Nb₅Si₃ and Laves Cr₂Nb phases exhibited variable ORs with respect to the Nb_SS phase. The Laves Cr₂Nb phase was found to play a negative role on the fracture toughness at room temperature and on the compressive strength at temperatures from 1523 K to 1623 K (1250 °C to 1350 °C). The fracture toughness and the compressive yield strength at 1623 K (1350 °C) both decreased from 14.4 to 10.3 MPa m^1/2 and from 300 to 85 MPa, respectively, when the nominal Cr content increased from 2 to 17 at. pct. Finally, the fracture modes of these typical Nb_SS/Nb₅Si₃ and Nb_SS/Nb₅Si₃/Cr₂Nb microstructures under bending and compression conditions at room and high temperatures were investigated and discussed.     

Study on Quantification of Oxide Phases in Ex-situ AlN/Al Metal Matrix Nanocomposites

Al based metal matrix nanocomposite (MMNC) is synthesized by dispersing nanocrystalline aluminium nitride (AlN) particles in Aluminum matrix using ex-situ melt metallurgy method. The entrapment of atmospheric oxygen along with ex-situ particulate has been a long standing issue during fabrication of metal matrix composites. In the present investigation, presence of oxygen has been quantified in synthesized Al-AlN MMNCs with varying AlN content. The high resolution scanning electron microscopy is used to study morphology and distribution of AlN in Al matrix. Energy dispersive spectroscopy analysis is used to quantify in situ oxide phases along with AlN particles in the synthesized MMNCs using thermodynamic mass balance calculations. Present study also attempts to understand the role of in-situ oxide phases on the mechanical properties of MMNCs using microindentation hardness and nanoindentation test.     

On the Transition of Internal to External Selective Oxidation on CMnSi TRIP Steel

The selective oxidation of a CMnSi transformation-induced plasticity (TRIP) steel during intercritical annealing (IA) in a N₂ + 10 pct H₂ gas atmosphere with a dew point (DP) in the range from 213 K to 278 K (?60 °C to +5 °C) was investigated by transmission electron microscopy. The decarburization during IA resulted in a fully ferritic matrix at the TRIP steel surface. Annealing in high DP gas atmospheres resulted in a reduction of the oxide layer thickness at the surface and an increase of the depth of the subsurface internal oxidation. The experimental results were compared to the calculations of the DP for the transition from internal to external oxidation based on the Wagner model. The evolution of the surface oxide composition during annealing was analyzed thermodynamically by means of the chemical potential diagram for the surface oxides. In the high DP atmosphere conditions, mainly, Mn-rich xMnO·SiO₂ (1 < x < 2) oxides were formed at the surface, while Si-rich xMnO·SiO₂ (x < 1) oxides were formed by internal oxidation. The use of a high DP gas atmosphere is therefore advantageous to induce internal selective oxidation and reduce the amount of surface oxides. It also leads to the formation of Mn-rich xMnO·SiO₂ (1 < x < 2) oxides.     

Corrosion Inhibition and Adsorption Behavior of Gentian Violet on AISI 4130 Alloy Steel in HCl Solution

The inhibition ability of hexamethyl pararosaniline chloride (gentian violet) on the corrosion resistance of AISI 4130 steel in 1 M HCl solution was studied by potentiodynamic polarization (Tafel), electrochemical impedance spectroscopy and scanning electron microscopy (SEM). Polarization studies indicated that the inhibition efficiency increases with the increase in inhibitor concentration and inhibitor retards both the cathodic and anodic reactions, so are classified as mixed type inhibitors. The effect of temperature on the corrosion behavior of steel in HCl with the addition of the inhibitor was studied in the temperature range from 25 to 65 °C. The experimentally obtained adsorption isotherms follow the Langmuir equation. Activation parameters and thermodynamic adsorption parameters of the corrosion process such as E _a , ΔH, ΔS, K _ads and ΔG _ads were calculated at different temperatures and using the adsorption isotherm. The morphology of steel surface after its exposure to HCl solution in the absence and presence of inhibitor was examined by SEM images.     

Stacking fault energy measurement from diffusion

The annealing kinetics of dislocation loops has been considered from climb theory based on a model involving vacancy diffusion as the rate controlling mechanism. The theory has been applied to fee metals of high, intermediate, and low stacking fault energy to determine both the intrinsic and extrinsic fault energy using transmission electron microscopy. Reliable values are obtained from metals with γ ? 70 erg per sq cm but for low γ metals the rate controlling mechanism is shown to be one of jog nucleation and propagation rather than vacancy diffusion. The technique of loop annealing is also shown to be applicable to hep metals such as zinc, magnesium, and cadmium, even when the foil surfaces act as vacancy sources. Results of loop shrinkage and loop growth are analyzed to provide fault energy values for those metals with hep structure.     

The Structure of Extruded NiAl

The deformation structure of Ni-rich NiAl extruded at 550°C has been characterized by transmission electron microscopy and by optical microscopy. Dislocations having a«100» Burgers vectors were found as complex networks, tangles, and prismatic loops. a«110» dislocations which were rare, were concluded to arise from reactions of a«100» dislocations. Evidence of recovery and recrystallization was obtained. Extrusion was deemed to have been possible by the operation ofhk0 «001» slip systems (often in plane strain flow) plus diffusion-assisted processes.     

Study of Structure and Deformation Pathways in Ti-7Al Using Atomistic Simulations,Experiments, and Characterization

Ti-7Al is a good model material for mimicking the α phase response of near-α and α+β phases of many widely used titanium-based engineering alloys, including Ti-6Al-4V. In this study, three model structures of Ti-7Al are investigated using atomistic simulations by varying the Ti and Al atom positions within the crystalline lattice. These atomic arrangements are based on transmission electron microscopy observations of short-range order. The elastic constants of the three model structures considered are calculated using molecular dynamics simulations. Resonant ultrasound spectroscopy experiments are conducted to obtain the elastic constants at room temperature and a good agreement is found between the simulation and experimental results, providing confidence that the model structures are reasonable. Additionally, energy barriers for crystalline slip are established for these structures by means of calculating the γ-surfaces for different slip systems. Finally, the positions of Al atoms in regards to solid solution strengthening are studied using density functional theory simulations, which demonstrate a higher energy barrier for slip when the Al solute atom is closer to (or at) the fault plane. These results provide quantitative insights into the deformation mechanisms of this alloy.     

The relationship between toughness and microstructure in Fe-high Mn binary alloys

The influence of Mn content on the ductile-brittle transition in 16 to 36 wt pct Mn steels was investigated and interpreted in light of the evolving microstructure. It was found that when hcp ε martensite is present in the as-quenched condition or forms during deformation, it lowers the toughness. In 25Mn steel, the stress concentrations at e plate intersections result in the formation of planar void sheets along the {111}_γ planes. The deformation-induced α’ martensite in 16 to 20 pct Mn alloys enhances the toughness, but leads to a ductile-to-brittle transition at low temperatures that is due to the intrusion of an intergranular fracture mode. Binary alloys with greater than 31 pct Mn also fracture in an intergranular mode at 77 K although the impact energy remains quite high. Auger spectroscopy of the fracture surfaces shows no evidence of significant impurity segregation, which suggests the importance of slip heterogeneity in controlling intergranular fracture in these alloys.     

Deformation of two C36 laves phases by microhardness indentation at room temperature

Microhardness indentation and electron microscopy were used to study the room-temperature deformation behavior of two Laves phases, ZrFe₂ and MgNi₂, in two-phase alloys. Evidence of extensive plastic deformation was found around the indentations. Activation of basal and nonbasal slip systems forms a distinctive cell structure in both Laves phases. Slip on planes nearly normal to the basal plane occurs in the lamellar form of ZrFe₂. Burgers vectors of the dislocations and resulting shear displacements are studied using high-resolution transmission electron microscopy (TEM). Curved or zigzag nonbasal slip surfaces in atomic scale were observed. Each slip plane can be considered to be composed of a series of small facets of high atomic density. A common Burgers vector and displacement vector component of 1/4 [0001] was found on many different slip planes. The “zonal glide” concept for slip on prismatic planes is discussed.