Crystal Specimens Research Articles

Creep rupture of smoothed and notched DD6 single crystal superalloy specimens subjected to high-temperature hot corrosion

This work studies the creep rupture behaviors of both smoothed and V-notched DD6 Ni-based single crystal superalloy specimens under both air and corrosion conditions, within a stress range of 300 to 700 MPa at 950 °C. The corrosive medium used consisted of a mixed salt containing 95 wt% Na2SO4 and 5 wt% NaCl. Experimental results revealed that notched specimens exhibited a creep rupture life extended by 6–16 times compared to smoothed specimens, with the extension becoming more pronounced as the stress concentration increased. High-temperature hot corrosion (HTHC) shortened the creep rupture time by up to 75 %. A significant HTHC-creep interactive effect was found through comparative creep experiments in air and corrosion conditions. The HTHC affected the fracture modes of the specimens, with factors such as the amount of salt infiltration into the superalloy, the corrosion duration, and specimen configurations playing critical roles. Microstructural analysis revealed that, compared with γ′ precipitates, γ matrix phase was more prone to creep damage and was more susceptible to corrosion.

Microstructural investigation of Au ion-irradiated Eu-doped LaPO4 ceramics and single crystals

Ceramics and single crystals of LaPO4 monazite doped with Eu(III) were irradiated with 14 MeV Au5+ ions at three different fluences. Changes to crystallinity, local coordination environments, and topography were probed using grazing-incidence X-ray diffraction (GIXRD), vertical scanning interferometry (VSI), scanning electron microscopy (SEM), Raman, and luminescence spectroscopy. GIXRD data of the ceramics revealed fluence dependent amorphization. A similar level of amorphization was detected for samples irradiated with 5 × 1013 ions/cm2 and 1 × 1014 ions/cm2, whereas the sample irradiated with the highest fluence of 1 × 1015 ions/cm2 appeared slightly less amorphous. VSI showed clear swelling of entire grains at the highest ion fluence, while more localized damage to grain boundaries was detected for ceramic samples irradiated at the lowest fluence. Single crystal specimens showed no pronounced topography changes following irradiation. SEM images of the ceramic irradiated at the highest fluence showed topological features indicative of grain surface melting. Raman and luminescence data showed a different degree of disorder in polycrystalline vs. single crystal samples. While changes to PO4 vibrational modes were observed in the ceramics, changes were more subtle or not present in the single crystals. The opposite was observed when probing the local Ln-O environment using Eu(III) luminescence, where the larger changes in terms of an elongation of the Eu-O (or La-O) bond and an increasing relative disorder with increasing fluence were observed only for the single crystals. The dissimilar trends observed in irradiated single crystals and ceramics indicate that grain boundary chemistry likely plays a significant role in the radiation response.

Operative slip systems and their critical resolved shear stresses in η-Fe2Al5 investigated by micropillar compression at room temperature

The plastic deformation behavior of single crystals of orthorhombic η-Fe2Al5 has been investigated by micropillar compression at room temperature as a function of crystal orientation and specimen size. Plastic flow is observed even at room temperature by the operation of six slip systems; (001)<010>, (001)<110>, (001)<130>, {22‾3}<110>, {311}<1‾03> and {301}<1‾03>. The CRSS values for the six identified slip systems are very high all in the range of 1.1∼1.5 GPa and do not vary much with specimen size. In the middle of the stereographic projection, the (001)<010>, (001)<110>, (001)<130> and {22‾3}[110] slip systems operate according to the relative Schmid factors with the similar CRSS values in the range of 1.08∼1.23 GPa. In orientations close to [001], the {311}<1‾03> slip system as well as the {301}<1‾03> slip system operate with a much higher CRSS values around 1.5 GPa, producing wavy slip traces due to the occurrence of frequent cross-slip among these slip planes. In orientations close to the [100]-[110]-[010] symmetry line, on the other hand, premature failure occurs without the operation of any slip systems, although, the Schmidt factor-wise, the {311}<1‾03> and {301}<1‾03> slip systems could operate. The selection of slip systems, their CRSS values and the possible dislocation dissociation modes are discussed based on the overlapped atomic volume that occurs during shear along the slip direction on the slip plane, taking into account the partial occupancies of Al atoms in the linear atomic chain along the orthorhombic c-axis direction.

Macroscopic experimental study and microscopic phenomenon analysis of damage self-healing in salt rock

Salt rock is characterized by a low porosity, low permeability and self-healing ability, and it is one of the most common materials used for underground energy storage and construction in underground nuclear waste repositories. Studying the healing of macroscopic cracks in salt rock under different conditions is important for ensuring the stability of the rock surrounding a salt cavern. To evaluate the healing ability and effect of cracks in salt rock at the macroscale, two tests were designed to directly assess the healing ability of salt rock by analyzing the tensile strength and permeability recovery of healed crack surface. Furthermore, the microstructure of the healed macroscopic fractures in salt rock was observed using scanning electron microscopy (SEM), and the microscopic mechanisms of salt rock damage healing were analyzed. (1) The results show that the presence of water is an important condition for the healing of cracks in salt rocks. Fully fractured salt rock cracks can heal at a low pressure of 160 kPa, and the uniaxial tensile strength of the healed specimens can reach a maximum of 121.1 kPa. It was found via computed tomography (CT) that a healed crack was still a weak surface in the whole specimen. (2) Increases in temperature, environmental humidity, and normal stress all promote the self-healing of salt rock fractures. Based on the experimental data, a model describing the evolution of salt rock damage healing variables with respect to temperature, humidity, and stress was established. It was also observed that the change in salt rock damage healing variables over time during the healing process can be represented by a first-order exponential decay function. (3) Using SEM, detailed micro healing experiments were conducted on NaCl single crystal and impurity-containing salt rock specimens. The healing characteristics of intracrystalline cracks and intercrystalline cracks were studied. It was observed that salt rock damage healing manifests at the microscopic level as the filling of microcracks and crack segmentation caused by grain growth. Additionally, the presence of a certain amount of impurities was found to promote the growth of internal structures that heal cracks within salt rock. These findings are of great significance for evaluating the stability and tightness of the surrounding rock of salt cavern reservoirs.

Very high cycle fatigue of a notched Ni-based single crystal superalloy at high temperature

A new notched geometry has been developed for ultrasonic fatigue testing of CMSX-4 single crystal Ni-based superalloy specimens at 1000 °C. Ultrasonic fatigue tests were carried out at 1000 °C, R = -1 and 20 kHz using this new geometry. Two competing crack initiation mechanisms were identified for the studied range of fatigue lives: internal crack initiation from a casting pore associated to a rough zone (RZ) formation and surface crack initiation assisted by oxidation. Failure modes associated to the identified fatigue crack initiation mechanisms are discussed. Comparing fresh fractographic evidence with available results from the literature, it is shown that fatigue crack nucleation and first stages of crack propagation seem to govern VHCF fatigue life.

Phase-field approach assisted solution heat treatment efficient design for novel multicomponent Co-based superalloys

Fast homogenization without incipient melting is the key to designing solution heat treatment (SHT) process for single crystal superalloys. In this paper, a multicomponent phase-field model coupled with solidus temperature is developed for dynamically tracking incipient melting temperature, TIM, of alloy during SHT. The simulation process runs completely automatically only by inputting the composition information of as-cast specimen. Based on the obtained TIM-time profile, the holding temperature and the time of SHT are determined. Applying this approach to Co–30Ni–11Al–4W–1Ta–4Ti–5Cr single crystal specimen, a gradual increased TIM from 1247 °C to 1293 °C within 72,000 s is obtained, and thus a stepwise SHT process with a short time of less than 20 h is designed. The experimental verification shows that after SHT, the segregation coefficient of the slowest diffusing element W decreased from more than 2 to 1.065, the content of harmful secondary phase has decreased to below 0.1%, and no incipient melting occurs.

Tensile and micro-compression behaviour of AISI 316L austenitic stainless steel single crystals at 20 °C and 300 °C: Experiments, modelling and simulations

The mechanical behaviour of 316L stainless steel single crystal is characterised at room temperature and 300°C. Elasticity moduli at room temperature are obtained with resonant ultrasound spectroscopy. Their dependence on temperature is calibrated with molecular dynamics simulations. The plastic behaviour is characterised by tensile tests on millimetre-sized single crystal specimens and compression tests on micrometre-sized single crystal specimens. A constitutive model of crystal plasticity based on dislocation density hardening at finite strains is developed and implemented in an open-source material subroutine compatible with several finite element (FE) and fast Fourier transform (FFT) solvers. Tensile curves at room temperature and 300°C are used to calibrate the interaction coefficients for self and coplanar dislocation interactions. The dislocation mean free path for obstacle dislocations and the annihilation distance are also calibrated. The calibrated model predicts tensile curves in excellent agreement with experimental data. In addition, the predicted plastic strain fields are in good agreement with the experimental fields obtained by digital image correlation. Semi-quantitative agreement between simulation and experimental data is obtained for micro-compression tests without further calibration of the model. Finally, an extension to polycrystals with grain size effects is finally proposed. The predicted strain hardening behaviour is compared with experimental data on stainless steel polycrystals.

A search for the upper bound of the cleavage energy of silicon crystal

Griffith barrier of 2γs is the accepted fracture energy under vacuum at crack initiation in brittle materials. It was shown recently, however, that the Griffith barrier is only the lower bound of that energy, while the upper bound was found to be about 60% higher. This bound was found in specimens having relatively short, straight but slightly curved, crack fronts, leading to the conclusion that ‘shorter is tougher’ and stronger than predicted by Griffith. In the current investigation, we attempted to explore further, experimentally, the upper bound of the cleavage energy. This was done by cleaving silicon crystal specimens along its two low-energy cleavage systems by generating shorter precracks. We discovered that the upper bound energy in silicon is over 3 times the Griffith barrier under air for the above-mentioned crack systems. This is much above the theoretical predictions of the lattice-trapping effect and atomistic simulations. We further confronted Griffith’s finding that σa0 = Const, which became a keystone in fracture since it defines the fracture toughness and fracture energy.

The secondary orientation effect of single crystal superalloy thin-wall specimens at 850 °C with [001] primary orientation

An interesting phenomenon is found in Nickel-based single crystal superalloy thin-wall specimens which have the same [001] primary orientation and different secondary orientation with [100], [210], and [110] at 850 °C. Generally, the testing of cylindrical samples exhibits similar creep and tensile properties regardless of their vertical orientation distribution due to the circumferential symmetry of their geometric structure. However, the 850 °C experimental results of thin-wall specimens with the same [001] primary orientation show a significant difference in tensile ductility and creep life when the secondary orientation is different. The mechanism of the secondary orientation effect is completely discussed by combining experiment, digital image correlation (DIC), and finite element modelling (FEM), which result from the strengthening effect of Lomer-Cottrel dislocations and the ability to coordinate plastic deformation in tensile, the shrinkage rate of cross-section caused by the single slip system ({111} <11-2>) and deviation from [001] with a small angle in creep.

Effects of high energy laser peening followed by pre-hot corrosion on stress relaxation, microhardness and fatigue life and strength of single crystal nickel CMSX-4® superalloy

This study investigated the stress relaxation and fatigue life and strength of laser peened single crystal nickel superalloy specimens following hot corrosion exposure and then fatigue testing compared to un-peened and shot peened specimens. The specimens were treated by conventional laser peening and a new cyclic laser peening plus thermal microstructure engineering process. Stress measurements by slitting showed the plastic penetration depth of laser peening exceeded shot peening by a factor of 24. Un-peened and peened specimens were exposed to sulphate corrosives at 700°C for 300 hours and then fatigue tested. Tests of five non-laser peened specimens all failed in low cycle fatigue regime whereas three identically tested laser peened specimens all achieved multi-million-cycle runout without failure, indicating fully consistent large benefit for life by laser peening. Additional tests showed fatigue strength improvement of 2:1 by laser peening.

Structure and properties of NdCuGa[formula omitted] single crystals

This manuscript reports on the structural and magnetic properties of NdCuGa3 using powder and single crystal X-ray diffraction (XRD), zero-field single crystal neutron diffraction, magnetization, and specific heat measurements. Our XRD on a single crystal specimen of NdCuGa3 confirmed that it crystallizes in the tetragonal BaNiSi3-type structure. A magnetic phase transition at TN= 3.3 K is assessed using specific heat and ac magnetic susceptibility measurements. No additional anomaly below TN down to 50 mK was detected by performing specific heat measurements. Neutron single crystal diffraction data collected at T= 300 mK confirm the antiferromagnetic phase below TN= 3.3 K with the propagation vector τ→= (0.2, 0, 0). Possible magnetic structure solutions of NdCuGa3 are discussed.

On the inherent strength of Cr23C6 with the complex face-centered cubic D84 structure

The deformation behavior of single crystals of Cr23C6 with the complex D84 crystal structure based on the face-centered cubic lattice has been investigated by micropillar compression as a function of crystal orientation and specimen size at room temperature. For the first time, the {111}<1‾01> slip system is identified to be the only operative slip system. The 1/2<1‾01> dislocation dissociates into two partial dislocations with identical collinear Burgers vectors (b) as confirmed by transmission electron microscopy (TEM) and atomic-resolution scanning transmission electron microscopy (STEM). The energy of the stacking fault bounded by two coupled partial dislocations with the b = 1/4<1‾01> is evaluated from their separation distances to be 840 mJ/m2. The critical resolved shear stress (CRSS) for {111}<1‾01> slip increases with the decrease in the specimen size, following the inverse power-law relationship with a relatively low exponent of ∼ -0.19. The room-temperature bulk CRSS value evaluated by extrapolating this inverse relationship to the specimen size of 20∼30 μm is 0.79 ± 0.15 GPa. The exact position of the slip plane among many different parallel {111} atomic planes and possible dislocation dissociations on the relevant slip planes are discussed based on the calculated generalized stacking fault energy (GSFE) curves. The inter-block layer slip is deduced to occur for {111}<1‾01> slip based on the TEM/STEM observations and the result of GSFE calculations. Finally, plausible atomic structures for stacking faults on (111) and coherent twin boundaries are discussed.

Toward single crystal nickel fabrication using WAAM – A first report

The present study is focused on investigating the feasibility of additive manufacturing of single crystal nickel components using MIG processed wire arc additive manufacturing (WAAM) technique. The feasibility was validated by depositing the material first on 99.999 % pure polycrystalline nickel substrate and then onto a 99.995 % pure single crystal nickel specimen oriented in <111> direction. Optical microscopy and EBSD results prove the possibility for regions of single crystal to be deposited. The process yielded distinct regions of single crystal. Columnar and equiaxed grains occurred in a region with the highest local thermal gradient and slowest solidification rate. EBSD analysis confirmed that the single crystal region revealed in optical microscopy was in one orientation and the etchant was effective in highlighting individual grain boundaries.

Room-temperature deformation of single crystals of WC investigated by micropillar compression

The room temperature deformation behavior of single crystals of WC has been investigated as a function of crystal orientation and specimen size by micropillar compression tests. Plastic flow is successfully observed at room temperature by the operation of slip on {011¯0}〈21¯1¯3〉 when the specimen size is reduced to micrometer orders. This slip system is the only operative slip system in WC at room temperature, and thus plastic flow is not observed for crystal orientations close to the c-axis orientation. The bulk critical resolve shear stress (CRSS) is estimated to be 1.2 ± 0.3 GPa from the extrapolation of the size-dependent CRSS. The 1/3〈21¯1¯3〉 dislocation carrying slip on {011¯0} dissociates into two identical collinear partial dislocations separated by a stacking fault with the energy of 211∼264 mJ/m2. The preference of slip along 〈21¯1¯3〉 among possible directions (such as 〈21¯1¯0〉 and [0001]) on the {011¯0} prism plane is discussed in terms of dislocation self-energy based on anisotropic elasticity, stacking fault energy, dislocation dissociation and Peierls stress for dislocation motion. The lowest Peierls stress arising from the shorter Burgers vector (1/6〈21¯1¯3〉) of dislocations as a result of collinear dissociation of dislocations with b = 1/3〈21¯1¯3〉 on the {011¯0} slip plane is considered to be the main reason for the preference of the {011¯0}〈21¯1¯3〉 slip system.

Processing of Single Crystal Aluminum Using Compacted Alumina Powder

This experiment was designed to produce single crystal aluminum specimens through the understanding of solidification and processing parameter effects. In order to conduct the experiment, specimens were prepared by steel die casting and machining. After aluminum specimens were machined and ground, they were placed in the center of a crucible. Alumina powder was then filled and compacted in the crucible. The crucible was placed in a furnace for the remelting process. Finally, it was placed on a heat sink and was allowed to solidify. The powder compacting methods and remelting temperature were the two most important processing parameters. They were modified to improve the test and create single crystal microstructure. It was found that the compacting methods significantly affected the formation of leak within the crucible. Extremely dense powder results in crack openings; extremely loose powder results in formation of branch-like leakages. Uniformly and gently compacted powder will optimize the result. Remelting temperature affects the amount of thermal expansion. High temperature results in large amount of expansion,and causes cracks in the powder. Low temperature requires much more time and it cannot be guaranteed that the specimen is completely melted. The grain size and microstructure of each trial was compared and analyzed. Necessary modification of procedure was also made to improve future results. Finally in the report, the processing parameters and the resulting microstructure were correlated and discussed.

In-situ TEM characterization of basal dislocations between nano-spaced long-period stacking ordered phases in MgYZn alloy

Long-period stacking ordered (LPSO) phases play strong barriers to the motion of non-basal dislocations and deformation twins, effectively improving the strength of Mg alloys. Corresponding to the crystallographic character of LPSO phases, it is generally believed that LPSO phases would not affect the motion of basal dislocations. Here, we perform in-situ TEM nanoindentation testing in a single crystal specimen of Mg97Y2Zn alloy that contains LPSO phases with various spacing within 100 nm, and report on a significantly low activity of basal dislocations in Mg matrix between LPSO phases with spacing less than 20 nm. Atomic HADDF-STEM results reveal a high concentration of solute atoms near LPSO phases, which could provide strong solute strengthening effect. These findings may provide possible guidance to design ultra-high strength of Mg alloys containing nano-spaced LPSO phases.

Capacitive discharge in flash experiments: A discussion of the charged species

AbstractWe report on the discharge of the capacitance formed at the electrodes in flash experiments with yttria stabilized zirconia. The experiments were carried out by disconnecting the current, and, instead, short circuiting the electrodes through a resistor. The time dependent voltage across the resistor was measured; the ratio yielded the discharge current. The current decayed exponentially with time, as expected in an RC circuit, which allowed the measurement of the capacitance. Experiments were carried out in two ways. In one case the specimens were flashed within a glove box filled with Ar (&lt; 1 ppm O2): these yielded electronic conductors. In the other case the specimens were flashed in ambient air: while electronically conducting in‐flash these specimens recover their prior insulating behavior as soon as the current is turned off. The stored charge was two orders of magnitude greater in the Ar experiments. Rather unexpectedly, the sign of the voltage expressed at the electrodes was opposite in experiments carried out in air and in Ar. The capacitance measured in the discharge experiments is attributed to the formation of space charge adjacent to the electrodes. In the case of Ar experiments, the capacitance is very large, approaching 1 F; in this case the space charge is expected to be constituted from ions. In the air experiments the specimen becomes insulating, trapping the electrons as a space charge. Hall effect measurements of the carrier density and X‐ray photoelectron spectroscopy characterization of electronically conducting single crystal specimen of cubic zirconia are reported.

Effects of temperature on critical resolved shear stresses of slip and twining in Mg single crystal via experimental and crystal plasticity modeling

Magnesium (Mg) single crystal specimens with three different orientations were prepared and tested from room temperature to 733 K in order to systematically evaluate effects of temperature on the critical resolved shear stress (CRSS) of slips and twinning in Mg single crystals. The duplex non-basal <a> slip took place in the temperature range from 613 to 733 K when the single crystal samples were stretched along the <01¯10> direction. In contrast, the single basal <a> slip and prismatic <a> slip were mainly activated in the temperature range from RT to 733 K when the tensile directions were inclined at an angle of 45° with the basal and the prismatic plane, respectively. Viscoplastic self-consistent (VPSC) crystal modeling simulations with genetic algorithm code (GA-code) were carried out to obtain the best fitted CRSSs of major deformation modes, such as basal <a> slip, prismatic <a> slip, pyramidal II <c+a>, {101¯2} tensile twinning and {101¯1} compressive twinning when duplex slips accommodated deformation. Additionally, CRSSs of the basal <a> and the prismatic <a> slip were derived using the Schmid factor (SF) criterion when the single slip mainly accommodated deformation. From the CRSSs of major deformation modes obtained by the VPSC simulations and the SF calculations, the CRSSs for basal <a> slip and {101¯2} tensile twinning were found to show a weak temperature dependence, whereas those for prismatic <a>, <c+a> slip and {101¯1} compressive twinning exhibited a strong temperature dependence. From the comparison of previous results, VPSC-GA modeling was proved to be an effective method to obtain the CRSSs of various deformation modes of Mg and its alloys.

Modeling and simulation of laser shock waves in elasto-plastic polycrystalline microstructures

We study the propagation of elasto-plastic shockwaves induced by high power laser impacts in 2D polycrystalline metallic alloys in order to investigate the influence of the material microstructure on the fields of plastic strain and subsequent residual stresses. Implementing a visco-plastic constitutive relation at the grain scale accounting for two dislocation slip systems into a finite volume numerical scheme, simulations on single crystal specimens with different lattice orientations show that plastic strain is concentrated in narrow bands originating at the edges of the laser impact and parallel to the slip planes. In the case of polycrystalline microstructures composed of randomly oriented grains, it is found that the microstructure morphology is the origin of a heterogeneous distribution of the residual plastic strain and stress fields, which thus departs from the residual stress fields usually modeled when the microstructure is not accounted for. To account for the random character of polycrystal microstructures, we perform a statistical analysis of the mechanical fields over a large number of microstructures to quantify the dispersion of the results. It is found that even though the residual stresses induced by a laser impact are in compression on average at the center of the laser impact, some realizations of the microstructures can lead to localized concentrations of less compressive, or even tensile, residual stresses at the surface, thus probably reducing the fatigue resistance of the shocked material.

Theoretical Basis for the Photoelastic Residual Stress Evaluation in Misaligned Cubic Crystals

Photoelasticity is a fast and powerful technique for internal stress detection and quality control in crystals; to fully exploit its possibilities, an appropriate theoretical analysis must be developed for different crystallographic structure and observation planes. For a cubic crystal specimen whose geometry is non-coherent with its crystallographic directions (i.e., observation planes and crystallographic directions are not parallel), we write a set of equations that allow an estimate of the refraction indices as a function of the residual stress. This is obtained upon the assumption that the residual stress may be represented by a plane stress parallel to the observation face. For cubic crystals, we obtain an explicit estimate of the residual stress intensity; this can be achieved provided we know the piezo-optic tensor component, the orientation of two non-parallel specimen faces with respect to the crystallographic axes, and that we can measure the principal directions of the refractive indices on the observation face.