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Report describes results of investigation of preparation, nucleation and controlled growth of particulate deposits (palladium and iron) on electron-transparent alumina substrates. Results indicate that characteristic properties of metal deposits are strongly dependent on cleanliness, phase, and crystallographic orientation of substrate.
A FIB/STEM interfacial study was performed on a TBC/Ti 2 AlC MAX phase system, oxidized in an aggressive burner rig test (Mach 0.3 at 1300 °C for 500 h). The 7YSZ TBC, α-Al 2 O 3 TGO, and MAXthal 211 TM Ti 2 AlC base were variously characterized by TEM/STEM, EDS, SADP, and HRTEM. The YSZ was a mix of “clean” featureless and “faulted” high contrast grains. The latter exhibited ferro-elastic domains of high Y content tetragonal t″ variants. No martensite was observed. The TGO was essentially a duplex α-Al 2 O 3 structure of inner columnar plus outer equiaxed grains. It maintained a perfectly intact, clean interface with the Ti 2 AlC substrate. The Ti 2 AlC substrate exhibited no interfacial Al-depletion zone but, rather, numerous faults along the basal plane of the hexagonal structure. These are believed to offer a means of depleting Al by forming crystallographic, low-Al planar defects, proposed as Ti 2.5 AlC 1.5 . These characterizations support and augment prior optical, SEM, and XRD findings that demonstrated remarkable durability for the YSZ/Ti 2 AlC MAX phase system in aggressive burner tests.
Transitions between phases and states of crystallographic order in films, noting conditions for preferential nucleation and analogies between two- and three-dimensional phase diagrams
Pure phases of some oxidized Ni oxides were prepared galvanimetrically with the Ni(2) hydroxide electrode of an alkaline battery. The crystallographic data of these phases, their chemical behavior, and conditions of transition were studied.
Recent studies of low-Z molecular materials including hydrogen to multimegabar pressures (less than 300 GPa) have uncovered a range of phenomena relevant to understanding the nature of the interiors of the outer planets and their satellites. Synchrotron x ray diffraction measurements (to 42 GPa) have been used to determine the crystal structure of the solid (hexagonal-close packed) and equation of state. Sound velocities in fluid and solid hydrogen (to 24 GPa) have been inverted to obtain elastic constants and aggregate bulk and shear moduli. In addition, an improved intermolecular potential has been determined which fits both static and shock-wave data. Use of the new potential for the molecular envelope of Jupiter suggests the need for major revisions of existing Jovian models or a reanalysis of reported free oscillations for the planet. Studies at higher pressures (greater than 100 GPa) reveal a sequence of pressure-induced symmetry-breaking transitions in molecular hydrogen, giving rise to three high-pressure phases (1, 2, and 3). Phase 1 is the rotationally disordered hcp phase which persists from low pressure to well above 100 GPa at high temperature (e.g., 300 K). Phase 2 is a low-temperature, high-pressure phase (transition at 100 GPa and 77 K in H2) with spectral features indicative of partial rotational ordering and crystallographic distortion. The transition to Phase 3 at 150 GPa is accompanied by a weakening of the molecular bond, gradual changes in orientational ordering, strong enhancement of the infrared intramolecular vibrational absorption, and strong intermolecular interactions similar to those of ambient-pressure network solids. Studies of the phase diagram reveal a triple point near 130 K and 160 GPa. Higher pressure measurements of vibrational spectra place a lower bound of approximately 250 GPa on the predicted transition pressure for dissociation of molecular hydrogen to form a monatomic metal.
The influence of microstructure on the fracture mechanism and plane-strain fracture toughness of Ti-5Al-2.5Sn was studied through the use of fractography and metallographic sectioning techniques. One-inch thick plates of extra low interstitial (ELI) and normal interstitial Ti-5Al-2.5Sn were mill annealed at 815 C followed by either air or furnace cooling. These variations in composition and cooling rate resulted in differences in the volume fraction and internal structure of the iron-stabilized phase, and in the crystallographic texture and ordering of the alpha matrix. The tensile properties of these plates were determined at 20 K, 77 K, and 295 K. The air-cooled ELI plate was the toughest material evaluated.
Eutectic rods of Al2O3 and Y3Al5O12 were grown by a laser-heated float zone method, and their microstructure and crystallographic texture were studied by scanning electron microscopy, electron backscattered diffraction and x-ray diffraction. The composites were found to be highly textured with two twin-related crystallographic orientation relationships between the phases. Electron backscattered diffraction was employed to determine the spatial distribution of the orientational variants within the samples and to define the crystallographic orientation of various microstructural features.
In order to better understand phase transformations, chemical migration, and isotopic disequilibrium in highly shocked rocks, we have performed a microprobe and an ATEM study on gneisses shocked up to 60 GPa from the Haughton Crater. This study reveals the following chemical and structural characteristics: (1) SiO2 dominant areas are formed by a mixture of pure SiO2 polycrystalline quartz identified by electron diffraction pattern and chemical analysis and a silica-rich amorphous phase containing minor amounts of aluminium, potassium, and iron; (2) Areas with biotitelike composition are formed by less than 200-nm grains of iron-rich spinels embedded in a silica-rich amorphous phase that is very similar to the one described above; (3) Layers with feldsparlike composition are constituted by 100-200-nm-sized alumina-rich grains (the indexation of the crystalline structure is under progress) and the silica-rich amorphous phase; (4) Zones characterized by the unusual Al/Si ratio close to 1 are formed by spinel grains (200-nm-sized) embedded in the same silica-rich amorphous phase; and (5) The fracturated sillimanites contain domains with a lamellar structure, defined by the intercalation of 100-nm-wide lamellae of mullite crystals and of a silica-rich amorphous phase. These mullite crystals preserved the crystallographical orientation of the preshock sillimanite. All compositional domains, identified at the microprobe scale, can thus be explained by a mixture in different proportion between the following phases: (1) a silica-rich amorphous phase, with minor Al and K; (2) quartz crystals; (3) spinel crystals and alumina-rich crystals; (4) sillimanite; and (5) mullite. Such mixtures of amorphous phases and crystals in different proportions explain disturbed isotope systems in these rocks and chemical heterogeneities observed on the microprobe.
A semi-empirical model has been developed to determine the complete crystallographic orientation dependence of the growth rate for vapor phase epitaxy (VPE). Previous researchers have been able to determine this dependence for a limited range of orientations; however, our model yields relative growth rate information for any orientation. This model for diamond and zincblende structure materials is based on experimental growth rate data, gas phase diffusion, and surface reactions. Data for GaAs chloride VPE is used to illustrate the model. The resulting growth rate polar diagrams are used in conjunction with Wulff constructions to simulate epitaxial layer shapes as grown on patterned substrates. In general, this model can be applied to a variety of materials and vapor phase epitaxy systems.
High-pressure minerals such as coesite, stishovite, and reidite are often used as indicators of shock metamorphism. However, high-pressure and high-temperature phases are metastable at ambient conditions and, therefore, often revert to a more energetically favorable phase. During solid-state transformations, the crystallographic orientations of the stable polymorph are controlled by the transformation pathway from the parent. Microstructural orientation analysis using electron backscatter diffraction (EBSD) of the stable phase can reveal systematic intercrystalline orientation relationships (OR) diagnostic of solid-state transformations from these high-pressure or high-temperature polymorph phases (Cayron et al., 2006). Knowledge of polymorph stability fields for a given system can thus be used to infer minimum shock P and/or T conditions that rocks have experienced, which are otherwise unavailable using traditional thermobarometers such as element partition coefficients. Using orientation relationships to infer the former presence of mineral phases has been termed microstructural “phase heritage”, and has successfully been used to probe for evidence of extreme pressures and temperatures resulting from hypervelocity impacts. The reconstruction of polymorphs of ZrSiO4 (zircon, reidite) and ZrO2 (baddeleyite) have further elucidated the behavior of these phases under hypervelocity impact conditions (Timms et al., 2017a; White et al., 2018), and OR analysis of shocked monazite has identified a previously unrecognized tetragonal high-P polymorph (Erickson et al., 2019). Zircon will convert to the low tetragonal polymorph reidite at shock stresses above ~21 GPa. However, upon decompression at temperatures above 1200 °C reidite will revert to zircon (Kusaba et al., 1985). Recrystallized zircon neoblasts encased in impact melt often show systematic misorientation relationships of 90° about <110> indicative of reversion from the reidite (Fig. 1), and preserving cryptic evidence of the high-P history that is often erased by the post shock thermal spike (Cavosie et al., 2016). Microstructural OR analysis of a dissociated zircon corona composed of baddeleyite (monoclinic-ZrO2) has identified the former presence of cubic zirconia within impact melt glass from the Mistastin Lake impact structure, Labrador, CA. Based on stability fields in the ZrO2-SiO2 binary phase diagram, cubic zirconia records thermal conditions in excess of 2370 °C at ambient P, indicating that the Mistastin impact melt is the hottest rock identified on Earth’s surface (Timms et al., 2017b). Shock-deformed monazite (monoclinic La,Ce,ThPO4) containing lamellae comprised of interlocking laths has been identified from the Haughton Dome impact structure, Nunavut, Canada and Nördlinger-Ries Crater, southern Germany. The lath-structured lamellae are composed of four systematic orientation variants, which OR analyses indicate originate from a tetragonal parent whereby the [010]monoclinic aligns with either [100] or [010]tetragonal (Erickson et al., 2019). These results highlight utility of microstructural phase heritage analyses for the identification of unstable high-P or high-T polymorphs that uniquely record the extremely transient shock conditions produced by hypervelocity impacts.
The intensity, relative stability and directional behavior in alternating field demagnetization of natural, saturation, thermal and spontaneous magnetization were studied for a variety of iron meteorites. Results show that remanence and relative stability increase from the coarser to the finer-grained samples. In addition, natural remanent magnetization coercivity spectra are found to soften with coarsening of the grain size. The link between fine structure and magnetization direction in octahedrites is also discussed. The combined effect of magnetocrystalline- and shape-anisotropy of the crystallographically ordered ferromagnetic kamacite alpha-phase renders the iron meteorites of little use for the study of ancient solar system fields.
Review, for the transition series oxides, of the Mattis and Lander model, which is one of electrons interacting with lattice vibrations (electron and phonon interaction). The model displays superconducting, insulating, and metallic phases. Its basic properties evolve from a finite crystallographic distortion associated with a dominant phonon mode and the splitting of the Brillouin zone into two subzones, a property of simple cubic and body centered cubic lattices. The order of the metal-insulator phase transition is examined. The basic model has a second-order phase transition and the effects of additional mechanisms on the model are calculated. The way in which these mechanisms affect the magnetically ordered transition series oxides as described by the Hubbard model is discussed.
Ceramics, for the most part, do not have inherently good tribological properties. For example friction coefficients in excess of 0.7 have been reported for silicon nitride sliding on silicon nitride or on bearing steel (ref. 1). High friction is always accompanied by considerable wear. Despite their inherently poor tribological properties, the high strength and high toughness of silicon nitride (Si3N4) ceramics has led to their successful use in tribological applications (refs. 1 to 4). The upper temperature limit for the application of Si3N4 as wear-resistant material is limited by reaction with the tribological environment (ref. 3). Silicon nitride is known to produce a thin silicon dioxide film with easy shear capability that results in low friction and low wear in a moist environment (ref. 5). At elevated temperatures, the removal of the reaction product that acts as lubricant causes the friction coefficient to increase and, consequently, the wear performance to become poor. New materials are sought that will have wear resistance superior to that of Si3N4 at elevated temperatures and in harsh environments. A new class of oxide ceramic materials has been developed with potential for excellent high-temperature wear resistance. The new material consists of a multicomponent oxide with a two-phase microstructure, in which the wear resistance of the mixed oxide is significantly higher than that of the individual constituents. This is attributed to the strong constraining effects provided by the interlocking microstructures at different length scales, to the large aspect ratio of the phases, to the strong interphase bonding, and to the residual stresses. Fretting wear tests were conducted by rubbing the new ceramic material against boron carbide (B4C). The new ceramic material produced a wear track groove on B4C, suggesting significantly higher wear resistance for the oxide ceramic. The new material did not suffer from any microstructural degradation after the wear test. The wear rate of the new ceramic material at 600 C was determined to be on the order of 10-10 mm3/N-m, which is 3 to 5 orders of magnitude lower than that for the current state-of-theart wear-resistant materials (Si3N4and B4C). The friction coefficient of the new ceramic materials is on the order of 0.4, which is significantly lower than that of silicon nitride. This new class of oxide materials has shown considerable potential for applications requiring high wear resistance at high temperatures and in harsh environments. New understanding of the wear behavior of ceramic materials is emerging as a result of the surprisingly high wear resistance of two-phase oxide ceramics. There is excellent potential for further improvements in the wear resistance of oxide ceramics through optimizing the microstructure and altering the crystallographic properties of specific oxide materials as a second phase to reduce the coefficient of friction at elevated temperatures.
GRCop-42 (Cu-4 at.% Cr-2 at.% Nb) is a copper-based alloy optimized for high temperature, high thermal conductivity applications such as regenerative cooled rocket engine liners. For this application, it is important to minimize contamination such as trace elements and ceramic inclusions. NASA initiated a series of ten builds by eight companies to assess the repeatability of GRCop-42 between vendors and machines. Utilizing inductively coupled plasma – atomic emission spectroscopy (ICP-AES) and energy dispersive spectroscopy (EDS) techniques allowed for identification of contaminants and quantification of their chemistry. In addition, additive manufacturing (AM) creates a unique microstructure that is often highly textured in the build (Z) direction. Electron backscattered diffraction (EBSD) was used to begin quantifying the degree of crystallographic texture in the copper matrix grains. It was also used to identify the crystallographic form of Cr2Nb, the main strengthening phase, present in the samples. Results showed the presence of ceramic inclusions, highly textured grains, and both the low and high temperature phases of Cr2Nb being present.
A microstructure-based FEM model that couples crystal plasticity, crystallographic descriptions of the B2-B19' martensitic phase transformation, and anisotropic elasticity is used to simulate thermal cycling and isothermal deformation in polycrystalline NiTi (49.9at% Ni). The model inputs include anisotropic elastic properties, polycrystalline texture, DSC data, and a subset of isothermal deformation and load-biased thermal cycling data. A key experimental trend is captured.namely, the transformation strain during thermal cycling is predicted to reach a peak with increasing bias stress, due to the onset of plasticity at larger bias stress. Plasticity induces internal stress that affects both thermal cycling and isothermal deformation responses. Affected thermal cycling features include hysteretic width, two-way shape memory effect, and evolution of texture with increasing bias stress. Affected isothermal deformation features include increased hardening during loading and retained martensite after unloading. These trends are not captured by microstructural models that lack plasticity, nor are they all captured in a robust manner by phenomenological approaches. Despite this advance in microstructural modeling, quantitative differences exist, such as underprediction of open loop strain during thermal cycling.
Meteorites formed under highly reducing conditions can incorporate substantial amounts of Si in solid solution in their metallic phases. In enstatite meteorites, reduced Si appears in shreibersite, perryite and, in variable amounts, in the kamacite, taenite, and tetrataenite. Microprobe bulk analysis of Si in Fe,Ni particles of aubrites show a large variation from grain to grain; this large compositional range has been attributed to local equilibrium conditions in the specific T and/or fO2 environments in which they are formed. Si concentrations are homogeneous in the kamacite; in contrast, the Ni-rich phases (taenite and tetrataenite) show a characteristic Si profile. Concentrations of this element in tetrataenite are substantially higher than in the adjacent kamacite, and decrease smoothly towards the center of the taenite grain, matching very closely the M-shaped profile of Ni. Other elements with similar distribution patterns are Ge and Cu. A satisfactory explanation for this behavior cannot be given in the absence of experimental data for the diffusion of Si between alpha and gamma-Fe alloys. However, two end-member possibilities can be envisioned: the distribution of Si between kamacite and taenite may be controlled by (1) the crystallographic structure or (2) the chemical composition of the host phases. These possibilities are explored.
Recent efforts suggest the possibility that crystallization, and liquid-liquid (L-L) phase transitions and critical phenomena are characteristics universal to all macromolecular solutions. Of particular interest to protein crystallographers are the predictions of a critical slowing of crystal growth and subsequent formation of nascent crystals at the L-L phase boundary. Herein, the effects of the L-L phase transition on both crystal growth rates and microcrystal formation are experimentally determined. In general, it was determined that critical slowing down of protein crystal growth rates occurred, as predicted. The L-L phase transition, however, had a net negative influence in the formation of nascent protein crystals. Although crystal nucleation was not induced by the L-L phase transition, it is considered that the phase behavior of macromolecular solutions can be universally defined.
The stages of a cratering event are considered together with four distinct magnetization volumes, taking into account the jetted material, the ejecta, the impact melt, and shock-compressed material which remains in situ. Shock classifications are discussed along with mineralogical aspects of shock remagnetization, the behavior of iron sulfides, defect cubic spinels, ilmenite-hematite series, the Fe-Ti-O system, alloys phases, and silicates. Remagnetization mechanisms considered include a first order reversible crystallographic transition in bcc iron-nickel, a second order Curie point transition in fcc iron-nickel, shock-induced anisotropy, and shock melting of iron containing silicates. Experimental results are reported together with a hypothetical crater model.