Recrystallization and grain growth of cold-rolled gold sheet

Recrystallization and grain growth of a cold-rolled gold sheet with 98 pct reduction in area (RA) were investigated with electron backscatter diffraction (EBSD) and X-ray diffraction (XRD). Gold with some dopants (Be, Ca, and La) was used in this research and its recrystallization temperature was 320 °C. Isothermal annealing experiments at 400 °C, 500 °C, and 600 °C were carried out for the cold-rolled gold sheet, and recrystallization texture was examined. In the cold-rolled gold sheet, α- and β-fibers were measured mainly and some shear texture components were found on the surface. Shear texture components remained on the surface for 2 hours at 400 °C and were consumed by other recrystallized grains after 24 hours at 400 °C. Microstructure and texture evolution during in-situ annealing at 400 °C were investigated from the cold-rolled state to the fully recrystallized state using EBSD. Most of the newly, recrystallized grains came from the deformed β-fiber regions and consisted of β-fiber, cube, and other random orientations.     

Crystallographic Texture and Volume Fraction of <Emphasis Type="Italic">α</Emphasis> and <Emphasis Type="Italic">β</Emphasis> Phases in Zr-2.5Nb Pressure Tube Material During Heating and Cooling

The phase transformations in an as-received Zr-2.5Nb pressure tube material were characterized in detail by neutron diffraction. The texture and volume fraction of α and β phases were measured on heating at eight different temperatures 373 K to 1323 K (100 °C to 1050 °C) traversing across the α/(α + β) and (α + β)/β solvus lines, and also upon cooling at 1173 K and 823 K (900 °C and 550 °C). The results indicate that the α-phase texture is quite stable, with little change in the {0002} and { 11[`2]0 } \left\{ {11\bar{2}0} \right\} pole figures during heating to 1123 K (850 °C). The β-phase volume fraction increased while a slight change in texture was observed until heating reached 973 K (700 °C). On further heating to 1173 K (900 °C), there appears a previously unobserved α-phase texture component due to coarsening of the prior primary α grains; meanwhile the transformed β-phase texture evolved markedly. At 1323 K (1050 °C), the α phase disappeared with only 100 pct β phase remaining but with a different texture than that observed at lower temperatures. On cooling from the full β-phase regime, a different cooldown transformed α-phase texture was observed, with no resemblance of the original texture observed at 373 K (100 °C). The transformed α-phase texture shows that the {0002} plane normals are within the radial-longitudinal plane of the pressure tube following the Burgers orientation relationship of (110)<sub>bcc</sub>//(0002)<sub>hcp</sub> and [[`1]11]_\textbcc //[11[`2]0]_\texthcp [\bar{1}11]_{\text{bcc}} //[11\bar{2}0]_{\text{hcp}} with a memory of the precursor texture of the primary α grains observed on heating at 1173 K (900 °C).     

Superplasticity in a thermomechanically processed High-Mg,Al-Mg alloy

Superplastic elongations in excess of 400 pct have been observed in tension testing at 573 K (300 °C) and strain rate έ= 2 × 10^-3 s^-1 for a thermomechanically processed Al-10.2 pct Mg-0.52 pct Mn alloy. The thermomechanical processing consists of solution treatment and hot working, followed by extensive warm rolling at 573 K (300 °C), a temperature below the solvus for Mg in the alloy. This processing results in a fine subgrain structure in conjunction with refined and homogeneously distributed β(Al₈Mg₅) and MnAl₆ precipitates. This structure does not statically recrystallize when annealed at 573 K (300 °C) but appears to recrystallize continuously during deformation at such a temperature and the resulting fine grain structure deforms with minimal cavitation. At temperatures above the Mg-solvus,e.g., 673 K (400 °C), recrystallization and growth occur readily resulting in rela tively coarser structures which deform superplastically but with extensive grain boundary sliding and cavitation. Formerly in Materials Group, Mechanical Engineering, Naval Postgraduate School Formerly Graduate Student in Mechanical Engineering, Naval Postgraduate School     

Improvement in Fatigue Strength of Biomedical β-type Ti–Nb–Ta–Zr Alloy While Maintaining Low Young’s Modulus Through Optimizing ω-Phase Precipitation

The improvement in fatigue strength, with maintenance of a low Young’s modulus, in a biomedical β-type titanium alloy, Ti–29Nb–13Ta–4.6Zr (TNTZ), by thermomechanical treatment was investigated. A short aging time at an ω-phase-forming temperature combined with severe cold rolling was employed. A fine ω phase is observed in TNTZ subjected to this thermomechanical treatment. Because the rolling texture of β phase is formed by cold rolling, such as the ω phase may be preferentially oriented to a direction that is effective for inhibiting the increase in Young’s modulus. The samples aged at 573 K (300 °C) for 3.6 ks and 10.8 ks after cold rolling exhibit a good balance between a high tensile strength and low Young’s modulus. In the case of the sample aged for 3.6 ks, the tensile strength is improved, although the fatigue strength is not improved significantly. Both the tensile strength and the fatigue strength of the sample aged for 10.8 ks are improved. This fatigue strength is the highest among the TNTZ samples used in the current and in previous studies with Young’s moduli less than 80 GPa.     

Precipitation in Two Al-Mg-Ge Alloys

Two Al-Mg-Ge alloys with compositions Al-0.87Mg-0.43Ge (at. pct) and Al-0.59Mg-0.71Ge (at. pct) were investigated and compared using high-resolution transmission electron microscopy, annular dark-field scanning transmission electron microscopy, and nano-beam electron diffraction. The alloys contained fine needle- and lath-shaped precipitates after aging at 473 K (200 °C) for 16 hours, which produced hardnesses similar to those measured in comparable Al-Mg-Si alloys. The β″ phase was not observed. Instead, hardness was achieved by β′-like and disordered precipitates in the Mg-rich alloy, and U1-like and disordered precipitates in the Ge-rich alloy. In all cases, the fine precipitates had structures containing an ordered near-hexagonal network of Ge atoms with a = b ≈ 0.4 nm, which could be visualized directly in annular dark-field mode. The network is very similar to the recently discovered Si network that relates all precipitate structures in the Al-Mg-Si alloys. The orientation of the precipitate unit cells and the Ge network relative to the Al matrix differed from what has been observed for β′ and U1 in the Al-Mg-Si system.     

Notched Tensile and Impact Fracture of Ti-15-3 Laser Welds

The notched tensile strength (NTS) and impact toughness of Ti-15V-3Cr-3Sn-3Al (β-type titanium alloy Ti-15-3) laser welds aged at temperatures ranging from 590 K to 866 K (317 °C to 593 °C) were determined, and the results were compared to those of unwelded Ti-15-3 plates aged at the same temperature. At a given aging temperature, α precipitates in welded specimens were finer and exhibited higher hardness than those in unwelded specimens. Among the tested specimens, the weld aged at 644 K (371 °C) was most susceptible to notch sensitivity. In those welds aged at or above 755 K (482 °C), the coarse columnar structure was prone to interdendritic fracture during notched tensile tests, which reduced the NTS of the weld relative to that of the unwelded plate aged at an equivalent temperature. Of the tested specimens, the weld that was not subjected to the postweld aging treatment possessed the highest impact toughness among the specimens.     

Microstructural study of the titanium alloy Ti-15Mo-2.7Nb-3Al-0.2Si (TIMETAL 21S)

A relatively new titanium alloy, TIMETAL 21S (Ti-15Mo-2.7Nb-3Al-0.2Si-0.15O (in wt pct)), is a potential matrix material for advanced titanium matrix composites for elevated temperature use. In order to develop a perspective on the microstructural stability of this alloy, the influence of several commonly used heat treatments on the microstructure of TIMETAL 21S was studied using optical and transmission electron microscopy (TEM). Depending on the specific thermal treatment, a number of phases, includingα,ω- type, and silicide, can form in this alloy. It was found that both recrystallized and nonrecrystallized areas could be present in the microstructure of an annealed bulk alloy, but the microstructure of annealed sheet alloy was fully recrystallized. The mixed structure of the bulk alloy, developed as a result of inhomogeneous deformation, could not be removed by heat treatment alone at 900 °C. Athermalω-type phase formed in this alloy upon quenching from the solution treatment temperature (900 °C). Silicide precipitates were also found in the quenched sample. Thermal analysis was used to determine theβ transus and silicide solvus as close to 815 °C and 1025 °C, respectively. In solution-treated and quenched samples, a high-temperature aging at 600 °C resulted in the precipitation ofα phase. The precipitation reaction was slower in the recrystallized regions compared to the nonrecrystallized regions. During low-temperature aging (350 °C), the ellipsoidalω-type phase persisted in the recrystallized areas even after 100 hours, whereas a high density ofα precipitates developed in the nonrecrystallized areas within only 3 hours. The observed behavior in precipitation may be related to the influence of substructure in the nonrecrystallized areas, providing for an enhanced kinetics during aging. Theα precipitates (formed during continuous cooling from the solution treatment temperature, low-temperature aging, and high-temperature aging) always obeyed the Burgers orientation relationship. With respect to the microstructure, TIMETAL 21S is similar to other solute-lean, metastableβ titanium alloys.     

Precipitation in a Cu-30 Pct Ni-1 Pct Nb alloy

Decomposition of a Cu-30 pct Ni-1 pct Nb alloy on aging in the range of 866 K (600°C) to 1073 K (800°C) was investigated. The initial decomposition, concomitant with age hardening, occurred through the precipitation of body centered tetragonal metastable Ni₃Nb-γ” precipitates on the 100 matrix planes. Equilibrium orthorhombicβ phase formed either through a grain boundary cellular reaction at low temperature (≤973 K (700°C)) or as Widmanstaettenplatelets on the 1ll planes at higher temperatures (≥1073 K (800°C)) with the following crystallographic relationship: (0l0)_β//111_γ [100]β//[1•11]_γ. Based on the observations, a schematic transformation sequence is presented.     

Effect of Annealing on Thermal Stability, Precipitate Evolution, and Mechanical Properties of Cryorolled Al 7075 Alloy

The effect of annealing on microstructural stability, precipitate evolution, and mechanical properties of cryorolled (CR) Al 7075 alloy was investigated in the present work employing hardness measurements, tensile test, X-ray diffraction (XRD), differential scanning calorimetry (DSC), electron backscattered diffraction (EBSD), and transmission electron microscopy (TEM). The solution-treated bulk Al 7075 alloy was subjected to cryorolling to produce fine grain structures and, subsequently, annealing treatment to investigate its thermal stability. The recrystallization of CR Al 7075 alloys started at an annealing temperature of 423 K (150 °C) and completed at an annealing temperature of 523 K (250 °C). The CR Al 7075 alloys with ultrafine-grained microstructure are thermally stable up to 623 K (350 °C). Within the range of 523 K to 623 K (250 °C to 350 °C), the size of small η phase particles and AlZr₃ dispersoids lies within 300 nm. These small precipitate particles pin the grain boundaries due to the Zener pinning effect, which suppresses grain growth. The hardness and tensile strength of the CR Al 7075 alloys was reduced during the annealing treatment from 423 K to 523 K (150 °C to 250 °C) and subsequently it remains constant.     

The effect of Cu additions on the precipitation kinetics in an Al-Mg-Si alloy with excess Si

The microstructural evolution during age hardening of a Cu-bearing Al-Mg-Si alloy has been investigated by the three-dimensional atom probe (3DAP) and transmission electron microscope (TEM) techniques, in order to clarify the effect of Cu on the initial age-hardening response. After 30 minutes of artificial aging at 175 °C, the alloy shows a significant increase in hardness. The TEM observations have revealed that very fine, needle-shaped β″ precipitates are formed in addition to spherical Guinier-Preston (GP) zones, whereas only the spherical GP zones are observed in the Al-Mg-Si ternary alloy using the same aging condition. The number density of the precipitates is significantly affected by the preaging conditions. The 3DAP analysis shows that the distribution of Cu atoms is uniform after 30 minutes of artificial aging at 175 °C, whereas Cu atoms are incorporated into the needle-shaped β″ precipitates after 10 hours of aging at 175 °C. Based on these microanalytical results, the effect of Cu additions on the age-hardening response of Al-Mg-Si alloys is discussed.     

Orientation relationship between β-Mn and L21 matrix in a Cu2MnAl alloy

In the as-quenched condition, the microstructure of the Cu₂MnAl alloy was L2₁ phase containing extremely fine L-J precipitates. This result is different from that reported by other workers in the as-quenched Cu₂MnAl alloy. When the as-quenched alloy was aged at 350 °C, γ-brass precipitates started to appear within the L2₁ matrix. The orientation relationship between the γ-brass and the L2₁ matrix was determined to be cubic to cubic. This result is consistent with that observed by other workers in the aged Cu-Mn-Al alloy. When the alloy was aged at 460 °C, the γ-brass precipitates disappeared and platelike β -Mn precipitates occurred within the L2₁ matrix. As the aging temperature was increased to 560 °C, the morphology of the β-Mn precipitates changed from platelike to granular shape. Electron diffraction examinations indicated that in spite of the morphology change the same orientation relationship between the β-Mn and the L2₁ matrix is maintained, and it could be best stated as follows:

On the precipitation-hardening behavior of the Al-Mg-Si-Cu alloy AA6111

The precipitation-hardening behavior of aluminum alloy AA6111 during artificial aging and the influence of prior natural aging on the aging behavior were investigated. The evolution of microstructure was studied using quantitative transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The evolution of the relative volume fraction of precipitates for the solution-treated alloy was determined using isothermal calorimetry and a new analysis based on the DSC technique. Quantitative TEM was also used to obtain the rate of precipitation of microscopically resolvable phases during aging at 180 °C. Three types of precipitates, i.e., unresolved Guinier-Preston (GP) zones, β″, and Q′, were found to form during aging at 180 °C. The evolution of yield strength was related to the evolution of microstructure. It was found that the high hardening rate during artificial aging for the solution-treated alloy is due to the rapid precipitation of the β″ phase. Natural aging prior to artificial aging was found to decrease the rate of precipitation of β″. The slow hardening rate for the naturally aged alloy was attributed to the slower nucleation and growth of β″ phase.     

Influence of various heat treatments on the microstructure of polycrystalline IN738LC

IN738LC is a modern, nickel-based superalloy utilized at high temperatures in aggressive environments. Durability of this superalloy is dependent on the strengthening of γ′ precipitates. This study focuses on the microstructural development of IN738LC during various heat treatments. The 1120 °C/2 h/accelerated air-cooled (AAC) solution treatment, given in the literature, already produces a bimodal precipitate microstructure, which is, thus, not an adequate solutionizing procedure to yield a single-phase solid solution in the alloy at the outset. However, the 1235 °C/4 h/water quenched (WQ) solution treatment does produce the single-phase condition. A microstructure with fine precipitates develops if solutionizing is carried out under 1200 °C/4 h/AAC conditions. Agings at lower temperatures after 1200 °C/4 h/AAC or 1250 °C/4 h/AAC or WQ conditions yield analogous microstructures. Agings below ∼950 °C for 24 hours yield nearly spheroidal precipitates, and single aging for 24 hours at 1050 °C or 1120 °C produces cuboidal precipitates. Two different γ′ precipitate growth processes are observed: merging of smaller precipitates to produce larger ones (in duplex precipitate-size microstructures) and growth through solute absorption from the matrix. Average activation energies for the precipitate growth processes are 191 and 350 kJ/mol in the ranges of 850 °C to 1050 °C and 1050 °C to 1120 °C, respectively, calculated using the precipitate sizes from microstructures in the WQ condition, and 150 and 298 kJ/mol in the analogous temperature ranges, calculated from precipitate sizes in the microstructures in the slow furnace-cooled condition.     

The Origin of Microstructural Diversity,Texture, and Mechanical Properties in Electron Beam Melted Ti-6Al-4V

An additive layer manufacture (ALM) technique, electron beam melting, has been used for the production of simple geometries, from prealloyed Ti-6Al-4V powder. Microstructure, texture, and mechanical properties achieved under standard operating conditions have been investigated. Three transitional regions are observed with a change in microstructural formation dependent on the thermal mass of deposited material. Prior β-phase reconstruction, from room temperature α-phase electron backscatter diffraction (EBSD) data, reveals a strong texture perpendicular to the build axis. Variation of build temperature within the processing window of 898 K to 973 K (625 °C to 700 °C) is seen to have a significant effect on the properties and microstructure of both as-deposited and hot isostatically pressed (HIP) samples.     

Precipitates in As-Cast and Heat-Treated ASTM F75 Co-Cr-Mo-C Alloys Containing Si and/or Mn

The effect of the addition of Si or Mn to ASTM F75 Co-28Cr-6Mo-0.25C alloys on precipitate formation as well as dissolution during solution treatment was investigated. Three alloys—Co-28Cr-6Mo-0.25C-1Si (1Si), Co-28Cr-6Mo-0.25C-1Mn (1Mn), and Co-28Cr-6Mo-0.25C-1Si-1Mn (1Si1Mn)—were heat treated from 1448 K to 1548 K (1175 °C to 1275 °C) for a holding time of up to 43.2 ks. In the case of the as-cast 1Si and 1Si1Mn alloys, the precipitates were M₂₃C₆-type carbide, η phase (M₆C-M₁₂C–type carbide), and π phase (M₂T₃X-type carbide with a β-Mn structure), while in the case of the as-cast 1Mn alloy, M₂₃C₆-type carbide and η phase were detected. The 1Si and 1Si1Mn alloys required longer heat-treatment times for complete precipitate dissolution than did the 1Mn alloys. During the solution treatment, blocky dense M₂₃C₆-type carbide was observed in all the alloys over the temperature range of 1448 K to 1498 K (1175 °C to 1225 °C). At the heat-treatment temperature of 1523 K (1250 °C), starlike precipitates with stripe patterns—comprising M₂₃C₆-type carbide and metallic face-centered-cubic (fcc) γ phase—were detected in the 1Si and 1Si1Mn alloys. A π phase was observed in the 1Si and 1Si1Mn alloys heat treated at 1523 K and 1548 K (1250 °C and 1275 °C) and in the 1Mn alloy heat treated at 1548 K (1275 °C); its morphology was starlike-dense. The addition of Si appeared to promote the formation of the π phase in Co-28Cr-6Mo-0.25C alloys at 1523 K and 1548 K (1250 °C and 1275 °C). Thus, the addition of Si and Mn affects the phase and morphology of the carbide precipitates in biomedical Co-Cr-Mo alloys.     

Correlation between Microstructures and Oxidation Resistance in Zr-Nb-Ti Alloys

Oxidation behavior of Zr-10Nb-10Ti and Zr-10Nb-20Ti (compositions are in atomic percent) alloys has been investigated in air between 300 °C and 700 °C. Higher Ti content in the alloy enhances the oxidation resistance. The calculated isotherms by PANDAT[1,2] show that 20Ti enters a three-phase (αZr-hcp, βNb-bcc, and βZr-bcc) region at 500 °C, while 10Ti alloy continues to be a two-phase (αZr and βNb) alloy until 550 °C and then enters the three-phase (αZr, βNb, and βZr) region. Both alloys have a single-phase βZr solid solution at 700 °C, which is detrimental for the oxidation resistance. The βNb phase greatly contributes to the oxidation resistance in these two alloys. The common oxidation products have been identified as TiO₂, ZrO₂, and Nb₂O₅. Both alloys suffer from pest oxidation at temperatures between 500 °C and 550 °C, respectively (20Ti and 10Ti), up to 700 °C. X-ray diffraction (XRD) indicates strong peaks for monoclinic structure of ZrO₂ at temperatures above 600 °C.     

Delamination Effect on Impact Properties of Ultrafine-Grained Low-Carbon Steel Processed by Warm Caliber Rolling

Bulk ultrafine-grained (UFG) low-carbon steel bars were produced by caliber rolling, and the impact and tensile properties were investigated. Initial samples with two different microstructures, ferrite-pearlite and martensite (or bainite), were prepared and then caliber rolling was conducted at 500 °C. The microstructures in the rolled bars consisted of an elongated UFG structure with a strong α-fiber texture. The rolled bar consisting of spheroidal cementite particles that distributed uniformly in the elongated ferrite matrix of transverse grain sizes 0.8 to 1.0 μm exhibited the best strength-ductility balance and impact properties. Although the yield strength in the rolled bar increased 2.4 times by grain refinement, the upper-shelf energy did not change, and its value was maintained from 100 °C to −40 °C. In the rolled bars, cracks during an impact test branched parallel to the longitudinal direction of the test samples as temperatures decreased. Delamination caused by such crack branching appeared, remarkably, near the ductile-to-brittle transition temperature (DBTT). The effect of delamination on the impact properties was associated with crack propagation on the basis of the microstructural features in the rolled bars. In conclusion, the strength-toughness balance is improved by refining crystal grains and controlling their shape and orientation; in addition, delamination effectively enhances the low-temperature toughness.     

Development of recrystallization textures in 0.08%C steel

The present work investigates the effect of cold deformation on the evolution of microstructure and textures during recrystallization in 0.08%C steel. The cold rolling texture consists of partial α-fiber (RD//〈110〉) and complete γ-fiber (ND//〈111〉) along with Goss ({110}〈001〉) and cube ({100}〈100〉}) texture components. The sharpness of α-fiber, γ-fiber and cube component increases with the increase in rolling reduction from 70 to 85% while that of Goss component decreases. After recrystallization (750 and 800°C), the textures were composed of α and γ-fiber along with significant Goss components. The strength of γ-fiber decreases after annealing. The presence of Goss component in recrystallization textures is attributed to preferential nucleation in {111}〈112〉 type deformed grains.