Microstructural evolution after creep in aluminum alloy 2618

The microstructural evolution of Al–2.24 Cu–1.42 Mg–0.9 Fe–0.9 Ni (AA2618) alloy after 195 °C/18 h aging, as well as after 180 and 240 °C/100 h creep, has been studied by transmission electron microscopy and high resolution electron microscopy (HREM). The Guinier–Preston–Bagaryatsky (GPB) zones/co-clusters, S″, S, and Al₉FeNi phases co-exist in the alloys after the 195 °C/18 h aging. After creep, precipitates become coarser and the transformation of GPB zones/co-clusters and S″ to S phase take place. A large number of GPB zones/co-clusters as those in aging state exist after 180 °C/100 h creep which possibly dynamically precipitates during the creep process. After the 240 °C/100 h creep, most of the precipitates are S variants with a few GPB zones and S″ phase. More dislocations appear upon which precipitate colonies form after creep. HREM images show that most of the early precipitates less than about 5 nm cannot exhibit perfect lattice image for the existence of stress. However, certain GPB/co-clusters possessing coherent relationship with the matrix can also be observed. HREM demonstrates that certain S particles viewed along [100]_S and [013]_S have classic orientation relationship with the matrix, and that those upon the dislocations depart from the standard orientation.     

Dislocation motion in the early stages of high-temperature low-stress creep in a single-crystal superalloy with a small lattice misfit

Dislocation configurations at different creep stages (1100 °C and 137 MPa) in a superalloy TMS-75(+Ru) were studied in transmission electron microscopy (TEM) and the movement path of these creep-produced dislocations could be fully illustrated. Due to the small value of γ/γ′ lattice misfit, these dislocations cannot glide in the horizontal γ matrix channels by cross slip, but they mainly move by climbing around the γ′ cuboids. In the primary stage, the dislocations first move by slip in the γ-matrix channels. When they reach the γ′ cuboids, they move by climbing along the γ′ cuboid surfaces. In the secondary creep stage, dislocation reorientation in the (001) interfacial planes happens slowly, away from the deposition orientation of 〈110〉 to the misfit orientation of 〈100〉. The velocity of the reorientation is lower and a perfect γ/γ′ interfacial dislocation network cannot be formed quickly. This factor results in a large creep rate of the alloy during the secondary creep stage. The path for dislocation motion during the early creep stages consists of the following sequences: (i) climbing along the γ′ cuboid surface, (ii) deposition onto the (001) γ/γ′ interfacial plane, and (iii) reorientation from the 〈110〉 direction to the 〈100〉 direction.     

Post-β″ phases and their influence on microstructure and hardness in 6xxx Al-Mg-Si alloys

Starting from solid solution (T4) or a condition with β″ precipitates (T6), three Al-Mg-Si alloys with similar total solute content (1.3 at%), but different Si/Mg ratios (2, 1.25 and 0.8) were isothermally heat-treated at 250 or 260°C and investigated by transmission electron microscopy. The result microstructure for all alloys and conditions consisted of metastable, needle-shaped precipitates growing along 〈100〉 directions in aluminium. Each of the phases β″-Mg₅Si₆, β′-Mg_1.8Si, U1-MgAl₂Si₂ and U2-MgAlSi could be identified as main precipitate in the alloy with its solute Si/Mg ratio closest to the same ratio in the composition of that particular phase: The highest Si content alloy produced coarse needles of the trigonal U1-phase coexisting with finer precipitates of hexagonal B′-phase. The most common phase in the Mg-rich alloy is coarse needles of hexagonal β′-type. The Si/Mg ratio of 1.25 in one alloy is similar to the Si/Mg ratio in β″. Here the microstructure changes from that of fine β″ needles to fine needles of the orthorhombic U2-phase. This material remains strongest during heat-treatment. Nucleation on dislocations, mainly by the B′-phase, was observed to be significant in the case of Si-rich alloys heat-treated from T4-condition.     

Creep behavior of INCOLOY alloy 617

The microstructural features of INCOLOY alloy 617 in the solution annealed condition and after long-term creep tests at 700 and 800 °C were characterized and correlated with hardness and creep strength. Major precipitates included (Cr,Mo,Fe)₂₃C₆ carbides and the δ-Ni₃Mo phase. M₆C and MC carbides were also detected within the austenitic grains. However, minor precipitates particularly γ′-Ni₃(Al,Ti) was found to play an important role. At different exposure temperatures, the microstructural features of the Ni–22Cr–12Co–9Mo alloy changed compared with the as-received condition. The presence of discontinuously precipitated (Cr,Mo,Fe)₂₃C₆ carbides and their coarsening until the formation of an intergranular film morphology could be responsible both for a reduction in rupture strength and for enhanced intergranular embrittlement. The fraction and morphology of the γ′-phase, precipitated during exposure to high temperature, also changed after 700 or 800 °C exposure. At the latter test temperature, a lower volume fraction of coarsened and more cubic γ′ precipitates were observed. These microstructural modifications, together with the presence of the δ-phase, detected only in specimens exposed to 700 °C, were clearly responsible for the substantially good creep response observed at 700 °C, compared with that found at 800 °C.     

Effect of rare earth element additions on the impression creep of Sn–9Zn solder alloy

Creep behavior of the Sn–9Zn–RE alloys containing 0.1, 0.25 and 0.5 wt.% rare earth (RE) elements was studied by impression testing and compared to that of the eutectic Sn–9Zn alloy. The tests were carried out under constant punching stress in the range 40–135 MPa and at temperatures in the range 298–420 K. Results showed that for all loads and temperatures, Sn–9Zn–0.25RE had the lowest creep rate, and thus the highest creep resistance among all materials tested. This was attributed to the formation of Sn–RE second phase precipitates which act as the main strengthening agent in the RE-containing Sn–Zn alloys. RE contents higher than 0.25 wt.%, resulted in a lower creep resistance due to a reduction in the volume fraction of Zn-rich phase caused by the formation of Sn–Zn–RE intermetallics. The average stress exponents of 6.8, 6.9, 7.1, 6.8 and activation energies of 42.6, 40.6, 43.0 and 44.9 kJ mol⁻¹ were obtained for Sn–9Zn, Sn–9Zn–0.1RE, Sn–9Zn–0.25RE, and Sn–9Zn–0.5RE, respectively. These activation energies were close to 46 kJ mol⁻¹ for dislocation climb, assisted by vacancy diffusion through dislocation cores in the Sn. This, together with the stress exponents of about seven suggests that the operative creep mechanism is dislocation climb controlled by dislocation pipe diffusion.     

Rotary bending high-cycle fatigue behavior of DD32 single crystal superalloy containing rhenium

Smooth and notched specimens of single crystal superalloy DD32 were subjected to rotary bending high-cycle fatigue (HCF) loading at different temperatures. The experimental results demonstrate that fatigue strengths of the smooth and notched specimens reach the maxima and the minimum notch sensitivity displays at 760 °C. DD32 alloy exhibits excellent HCF properties compared to SRR99 alloy under the same test condition. As for the smooth specimens, slip bands moving through γ and γ′ phases as well as dislocation bowing are the main deformation modes. As for the notched specimens, the deformations are carried out by dislocation loop bowing and shearing of PSBs mode at intermediate temperatures; at 900 °C, the minimum fatigue strength results from dislocation climbing deformation and the degradation of γ′ precipitates. The fine secondary γ′ precipitates advantage the recovery of dislocations and further deformation of the fatigue specimens.     

L1<Subscript>2</Subscript>-phase cutting during high temperature and low stress creep of a Re-containing Ni-base single crystal superalloy

In the present study, we investigate dislocation processes in a Ni-base single crystal superalloy (LEK94) after high temperature and low stress creep. Specimens were creep deformed at 240 MPa and 980 °C to a strain of 20%. We use diffraction contrast transmission electron microscopy (TEM) to show that two γ-channel dislocations with different Burgers vectors combine and form a super dislocation that shears the γ′-particle. This type of cutting event has now been observed for three single crystal superalloys with different alloy chemistry (CMSX-4, CMSX-6 and LEK94 in the present work) and we therefore conclude that it represents a generic elementary dislocation process which governs high temperature (around 1000 °C) and low stress (around 240 MPa) creep. The present paper provides microstructural evidence for this type of cutting processes and discusses the results in the light of previous work published in the literature.     

The enhancement of creep in Al–22?wt% Ag alloy by cyclic stressing

The plastic deformation behavior of Al–22 wt% Ag alloy during phase transformation was investigated by studying the creep behavior under cyclic stress reduction of low frequencies. The cyclic creep curves obtained describe clearly the cyclic stress acceleration behavior. Increasing frequency of cyclic stress reduction enhanced the creep deformation depending upon the combination of the experimental variables as testing temperature, aging temperature and static creep rate. The irregularity in the creep parameters, n, β and ε_st with increasing aging temperatures, has been explained on the basis of structure transformations occurring in Al–Ag system and their mode of interaction with mobile dislocations.     

Frequency-dependent dielectric and electric modulus properties of Li–Ni–Sm–Fe–O spinel embedded in conducting polymer

Conducting polymeric nanocomposite containing Li–Ni–Sm–Fe–O spinel was synthesized by the chemical oxidizing of aniline in the presence of LiNi_0.5Sm_0.08Fe_1.92O₄ particles. The dielectric and electric modulus properties of the as-prepared samples were investigated over a frequency range from 10⁶ to 10⁹ Hz. The dielectric constant (ε′), dielectric loss (ε″) and dissipation factor (tan δ) for all samples presented relatively high values at low frequency and were found to decrease with the frequency. The values of ε′, ε″ and tan δ of the nanocomposite were lower than that of the pristine PANI. Electric modulus analysis had been carried out to understand the electrical relaxation process. The dielectric relaxation time for the nanocomposite became longer due to the introduction of LiNi_0.5Sm_0.08Fe_1.92O₄ particles lowering the crystallinity of PANI.     

Impedance spectroscopy analysis of double perovskite Ho<Subscript>2</Subscript>NiTiO<Subscript>6</Subscript>

The electrical properties of double perovskite Ho₂NiTiO₆ (HNT) are investigated by impedance spectroscopy in the temperature range 30–420 °C and frequency range 100 Hz to 1 MHz. The X-ray diffraction analysis reveals that the compound crystallizes in monoclinic phase. The imaginary part of impedance (Z″) as a function of frequency shows Debye type relaxation. The frequency dependence of Z″ peak is found to obey an Arrhenius law with an activation energy of 0.129 eV. Impedance data presented in the Nyquist plot (Z″ vs. Z′) are used to identify an equivalent circuit and to know the bulk and interface contributions. The complex impedance analysis of HNT exhibits the appearance of both the grain and grain-boundary contribution. The results of bulk ac conductivity as a function of temperature and frequency are presented. The activation energy (0.129 eV), calculated from the slope of log τ versus 10³/T plot, is found to be the nearly same as calculated (0.130 eV) from dc conductivity. The frequency dependent conductivity spectra obey the power law.     

Dielectric relaxation behaviour of Sr<Subscript><Emphasis Type="Bold">2</Emphasis></Subscript>SbMnO<Subscript><Emphasis Type="Bold">6</Emphasis></Subscript> ceramics fabricated from nanocrystalline powders prepared by molten salt synthesis

Double perovskite polycrystalline single phase and dense Sr ₂ SbMnO ₆ (SSM) ceramics, fabricated using the nanocrystalline powders synthesized by molten salt method, exhibited high dielectric constant with low dielectric loss as compared to that of SSM ceramics obtained from the powders prepared by solid-state synthesis method. The dielectric data obtained over a wide frequency (100 Hz–1 MHz) and temperature (190 K–300 K) ranges exhibited distinct relaxations owing to both the grain and grain boundary. The dielectric dispersion was modeled using the Cole–Cole equation consisting of two separate relaxation terms corresponding to the grain and grain boundary. The grain and grain boundary relaxations observed in the Nyquist plots (Z ^′ and Z ^″) were modeled by an equivalent circuit consisting of two parallel RC circuits connected in series with each other. A careful analysis of both the impedance (Z ^″ vs ω) and modulus (M ^″ vs ω) behaviour corroborated the conclusions drawn from the dielectric data.     

Dislocation configurations and internal stresses in the creep of Nimonic 91

The internal stress, σ_i, developed during the creep of Nimonic 91 was determined as a function of applied stress, σ_a, using the strain transient dip technique. Transmission electron microscope observations of thin films of crept specimens showed Orowan dislocation loops to exist aroundγ′ phase particles at low stresses with partial dislocation loops around faultedγ′ particles at high stresses. The numbers of loops per specimen volume were counted and the resulting internal stress calculated. The results indicate that a significant part of the mechanically measured internal stress can be attributed to Orowan loops aroundγ′ particles which are stabilized against climb by the superlattice fault resulting from partial penetration of theγ′ particle by the dislocation. The variation of internal stress with applied stress can be accounted for qualitatively by the variation of loop density with stress at low stresses and the initiation of relaxation processes involving partial or complete shearing ofγ′ particles by loops at high stresses. It is suggested that creep in Nimonic 91 is dependent on the magnitude of the effective (σ_a-σ_i) and that the internal stress is determined largely by the density of dislocation loops aroundγ′ particles.     

Mechanical properties of Cu–Cr system alloys with and without Zr and Ag

The effects of addition of Zr and Ag on the mechanical properties of a Cu–0.5 wt%Cr alloy have been investigated. The addition of 0.15 wt%Zr enhances the strength and resistance to stress relaxation of the Cu–Cr alloy. The increase in strength is caused by both the decrease in inter-precipitate spacing of Cr precipitates and the precipitation of Cu₅Zr phase. The stress relaxation resistance is improved by the preferentially forming Cu₅Zr precipitates on dislocations, in addition to Cr precipitates on dislocations. The addition of 0.1 wt%Ag to the Cu–Cr and Cu–Cr–Zr alloys improves the strength, stress relaxation resistance and bend formability of these alloys. The increase in strength and stress relaxation resistance is ascribed to the decrease in inter-precipitate spacing of Cr precipitates and the suppression of recovery during aging, and to the Ag-atom-drag effect on dislocation motion. The better bend formability of the Ag-added alloys is explained in terms of the larger post-uniform elongation of the alloys.     

Electrical conductivity and dielectric properties of cadmium thiogallate CdGa<Subscript>2</Subscript>S<Subscript>4</Subscript> thin films

Cadmium thiogallate CdGa₂S₄ thin films were prepared using a conventional thermal evaporation technique. The dark electrical resistivity calculations were carried out at different elevated temperatures in the range 303–423 K and in thickness range 235–457 nm. The ac conductivity and dielectric properties of CdGa₂S₄ film with thickness 457 nm has been studied as a function of temperature in the range from 303 to 383 K and in frequency range from 174 Hz to 1.4 MHz. The experimental results indicate that σ_ac(ω) is proportional to ω ^s and s ranges from 0.674 to 0.804. It was found that s increases by increasing temperature. The results obtained are discussed in terms of the non overlapping small polaron tunneling model. The dielectric constant (ε′) and dielectric loss (ε″) were found to be decreased by increasing frequency and increased by increasing temperature. The maximum barrier height (W _m) was estimated from the analysis of the dielectric loss (ε″) according to Giuntini’s equation. Its value for the as-deposited films was found to be 0.294 eV.     

Dielectric characteristic and local phase transition of gallium phosphide nanosolid

The dependences of relative dielectric permittivity, ε′ _r, and tangent of dielectric loss angle, tg δ, of gallium phosphide (GaP) nanosolid on frequency and temperature were investigated. The GaP nanopowders are subglobular in shape, with the average crystallite size of about 50 nm evaluated from Scherrer equation. It can be concluded that the leakage current mechanism plays an important role in the dielectric loss of the GaP nanosolid. The dielectric characteristic of the GaP nanosolid in the range 298–350 K allows to detect an ε′ _r or tg δ peak at 303 K that is due to local phase transitions, probably in the high hydrostatic stress field of dislocations with an edge component. Under the influence of an electric field, the high hydrostatic stress field of dislocations can undergo changes in deformation, accompanied by drastic stress-induced changes in the order parameter near the phase transition temperature, and hence, changes in the Gibbs free energy per unit volume can be found.     

Controllable synthesis and morphology-dependent microwave absorption properties of iron nanocrystals

Iron nanospheres, nanoflakes and nanofibers were synthesized via a simple pyrolysis method. When the pyrolysis temperature increased from 523 to 623 K and the flow rate of Ar carrier gas maintained at 100 sccm, the as-prepared iron nanocrystals showed a morphology evolution from isotropic nanospheres to isotropic nanofibers. The phase structures and morphologies of the composite were characterized by X-ray diffraction and scanning electron microscopy. The complex permittivity (ε′ − jε″) and permeability (μ′ − jμ″) of these composites were measured using the transmission/refection coaxial line method in the frequency range of 1–18 GHz by a vector network analyzer. The iron nanofibers exhibited superior microwave absorbing properties compared to iron nanoparticles and nanoflakes. The optimal reflection loss (RL) reached −17.8 dB at 9.9 GHz with a layer thickness of 2.0 mm. The RL below −10 dB can be obtained in the frequency range of 7.3–11.7 GHz. Considering the low cost and high efficiency; the iron nanofibers are favorable for application as microwave absorber.     

Precipitation behaviour of Al-Mg-Si alloys with high silicon content

The precipitation behaviour of three Al-Mg-Si alloys has been studied by differential scanning calorimetry (DSC) and transmission electron microscopy. Seven exothermic peaks are usually observed in DSC thermograms of Al-Mg-Si alloys with high silicon contents. These peaks are believed to be caused by the formation of clusters of silicon and magnesium atoms, Guinier-Preston zones, small precipitates with an unknown structure, β″ phase, B′ phase, silicon precipitates and β phase. The silicon content has no obvious effect on the precipitation of β″ and B′ phases in these alloys, but it has a pronounced influence on the formation of silicon precipitates. The cold-rolling reduction before solution heat treatment is also found to affect the precipitation process appreciably. This revised version was published online in November 2006 with corrections to the Cover Date.     

An investigation on electrical properties of microwave treated natural ilmenite (FeTiO3)

It has been observed that microwaves of 2.45 GHz heat dielectric materials. On subjecting natural ilmenite to microwave irradiation, the mineral is observed to heat, with a surface temperature in proportion to the irradiation time. With irradiation times from 40 to 240 seconds (increased in steps of 40 sec), the surface temperature measured on the samples were between 280 and 520 K. Electrical measurements made on the samples before and after irradiation show that the electrical properties are modified by the microwave irradiation. The real conductivity (σ′), dielectric constant (ɛ′) and the dielectric loss (ɛ″) plotted against frequency generally showed universal dielectric behaviour [1 and references therein] similar to that observed in other systems studied in the literature but using conventional heating techniques. Plots of σ′, ɛ′ and ɛ″ against the surface temperature of the sample showed frequency independent peaks around 460 K. The experimental dielectric loss (ɛ″) results fit a peak function of the form:

High temperature deformation behavior of permanent casting AZ91 alloy with and without Sb addition

The elevated temperature deformation behavior of permanent cast magnesium alloy AZ91 with and without Sb addition has been investigated using slow strain rate (5.0 × 10^–4s^–1) elevated temperature tensile and constant load creep testing at 150°C and 50 MPa. The alloy with 0.4 wt% Sb showed a higher elevated temperature tensile strength and creep resistance due to the formation of thermal stable Mg₃Sb₂ precipitates and a smaller microstructure as well as the suppressing of the discontinuous precipitation. Plastic deformation of AZ91 based alloys is determined by motion of dislocation in basal plane and non-basal slip systems. The dislocation motion in a slip system is influenced by temperature, precipitates and other lattice defects. Dislocations jog, grain boundaries and/or precipitates are considered as obstacles for moving dislocations. The deformation twinning were founded in the creep process by TEM. Cross slip of dislocations was taken into account as the main softening mechanism for permanent cast AZ91 alloy during elevated temperature deformation process.