Seeding of single crystal superalloys--Role of seed melt-back on casting defects

Single crystal seeds of the nickel-base superalloy CMSX-4 have been partially melted in a temperature gradient and then quenched. Small islands of random orientation are observed throughout the melted-back semi-solid. These random orientations appear to be pinched-off secondary dendrite arms, but there is no evidence that they are transported ahead of the dendrite tips to nucleate stray grains during directional solidification.

Evaluation of selective growth in a Fe-2.8% Si single crystal using Rodrigues-Frank space

A Fe-2.8%Si single crystal was scratched in order to randomise the texture in the neighbourhood of the notch. Annealing resulted in recrystallization and grain growth starting from the deformed zone. Misorientations between the single crystal matrix and the grown grains were gathered and were studied in order to investigate the possibility for selective growth based on a specific misorientation. However, instead of studying the misorientation angle or axis profiles separately in a 1D or 2D projection a full misorientation analysis was carried out in the 3-dimensional Rodrigues-Frank misorientation space, which offers an unambiguous interpretation of the data because no features are hidden or masked by a projection. It is concluded that the selective growth phenomenon following the <110>26.5deg misorientation relationship is strongly supported by the gathered orientation data, after appropriately normalizing these data with respect to a random misorientation distribution.

Large-scale synthesis and growth mechanism of single-crystal Se nanobelts

Single-crystal trigonal (t) Se nanobelts have been synthesized on a large scale by reducing SeO2 with glucose at 160 °C. Electron microscopy images show that the nanobelts are 80 nm in diameter, 25 nm in thickness, and up to several hundreds of micrometers in length. HRTEM images prove that the nanobelts are single crystals and preferentially grow along the [001] direction. The time-dependent TEM images revealed that the formation and growth of t-Se nanobelts were governed by a solid−solution−solid growth mechanism. The redox reaction directly produced amorphous (α) Se nanoparticles under hydrothermal conditions. t-Se nanobelts were formed by dissolution and recrystallization of the initial α-Se nanoparticles under the functional capping of poly(vinylpyrrolidone) (PVP). The nanobelts obtained exhibit a quantum size effect in optical properties, showing a blue shift of the band gap and direct transitions relative to the values of bulk t-Se.

Secondary bonding in para-substituted diphenyltellurium dichlorides (p-XC6H4)2TeCl2 (X = H, Me, MeO) probed by 125Te MAS NMR spectroscopy. Crystal and molecular structure of (p-MeC6H4)2TeCl2

The solid-state structures of the previously known para-substituted diphenyltellurium dichlorides, (p-XC₆H₄)₂TeCl₂ (X=H (1), Me (2), MeO (3)) were investigated by ¹²⁵Te MAS NMR spectroscopy and in case of 2 by single crystal X-ray diffraction. The ¹²⁵Te-NMR shielding anisotropy (SA) was studied by tensor analyses based on relative intensities of the observed spinning sidebands. Solid-state NMR parameters, namely the isotropic chemical shift (δ_iso), anisotropy (ζ) and asymmetry (η), were discussed in relation to the molecular structures established by X-ray crystallography. The asymmetry (η) was found to be particularly sensitive to structural differences stemming mostly from the diverse secondary Te...Cl interactions, but no correlation with geometric parameters could be established.

Effect of orientation stability on recrystallization textures of deformed aluminium single crystals

High purity Al single crystals of the Cube (0 0 1)[1 0 0] and rotated Cube (0 1 1)[0 1 ¯ 1] orientations have been deformed in plane strain compression in a channel die. Deformation was carried out at temperatures between 25 and 600 8C up to strains of 1.2. The as-deformed microstructure has been characterised using electron microscopy and electron backscattered diffraction (EBSD).
Annealing was carried out for various times and temperatures. The recrystallized microstructure has been studied using electron microscopy, and the orientation of recrystallized grains determined using EBSD. After cold deformation and annealing both orientations exhibited a random recrystallization texture component. After hot deformation both orientations retained a similar annealing texture to their starting deformation texture. The annealing texture of deformed single crystals was found to be more sensitive to the temperature of deformation than the stability of the orientation.

Conductivity, NMR and crystallographic study of N,N,N,N-tetramethylammonium dicyanamide plastic crystal phases : an archetypal ambient temperature plastic electrolyte material

N,N,N,N-Tetramethylammonium dicyanamide (Me₄NDCA) has been examined via differential scanning calorimetry (DSC), thermogravimetric analysis, conductivity, single crystal X-ray diffraction and ¹H nuclear magnetic resonance (NMR) analyses, and was found to be highly conductive in the solid state (σ =10−3 S cm⁻² at 420 K) and to also exhibit unusual plastic crystal behaviour. To investigate the correlation between such behaviour and the occurrence of molecular rotations in the crystal, ¹H NMR second moment measurements are compared with calculated values predicted from the crystal structure. While DSC analysis indicates a number of solid–solid transitions at ambient temperatures, subsequent ¹H NMR analysis of the Me₄N⁺ cation shows that a variety of rotational motions become active at low (<240 K) temperatures, and that such transitions in rotational states occur over a range of temperatures rather than in a sharp transition. Conductivity analysis reveals that between 320 K and 420 K the conductivity increases by more than six orders of magnitude in the solid state, in line with the transition of the Me₄N⁺ cation to a diffusive state, and that other phase transitions observed in this temperature range have no marked effect on the conductivity. Conduction in this solid state is therefore envisaged to involve a vacancy-diffusion model, involving Me₄N⁺ cation vacancies.

Symmetrically tapered <30-micron-thick quasi-planar Ge waveguides as chemical sensors for microanalysis

Symmetrically tapered planar IR waveguides have been fabricated by starting with a ZnS coated concave piece of single-crystal Ge, embedding it in an epoxide resin as a supporting substrate, and then grinding and polishing a planar surface until the thickness at the taper minimum is <30 μm. Such tapering is expected to enhance a waveguide's sensitivity as an evanescent wave sensor by maximizing the amount of evanescent wave energy present at the thinnest part of the waveguide. As predicted by theory, the surface sensitivity, i.e., the absorbance signal per molecule in contact with the sensing region, increases with decreasing thickness of the tapered region even while the total energy throughput decreases. The signal-to-noise ratio obtained depends very strongly on the quality of the polished surfaces of the waveguides. The surface sensitivity is superior to that obtained with a commercial Ge attenuated total reflection (ATR) accessory for several types of sample, including thin films (<10 ng) and small volumes (<1 μL) of volatile solvents. By using the waveguides, light-induced structural changes in the protein bacteriorhodopsin were observable using samples as small as ∼50 pmol (∼1 μg). In addition, the waveguide sensors can reveal the surface compositions on a single human hair, pointing to their promise as a tool for forensic fiber analysis.

Direct measurement of surface forces between sapphire crystals in aqueous solutions

Measurements are presented of the electrical double layer and van der Waals forces between the (0001) surfaces of two single-crystal sapphire platelets immersed in an aqueous solution of NaCl at pH values from 6.7 to 11. The results fit the standard Deryaguin-Landau-Verwey-Overbeek (DLVO) theory, with a Hamaker constant of 6.7 × 10−20 J. These are the first measurements made using the Israelachvili surface forces apparatus without mica as a substrate material, and they demonstrate the possibility of using this technique to explore the surface chemistry of a wider range of materials.

Effects of crystallographic orientation on corrosion behavior of magnesium single crystals

The corrosion behavior of magnesium single crystals with various crystallographic orientations was examined in this study. To identify the effects of surface orientation on the corrosion behavior in a systematic manner, single-crystal specimens with ten different rotation angles of the plane normal from the [0001] direction to the [1010] direction at intervals of 10° were prepared and subjected to potentiodynamic polarization and potentiostatic tests as well as electrochemical impedance spectroscopy (EIS) measurements in 3.5 wt.% NaCl solution. Potentiodynamic polarization results showed that the pitting potential (E _pit) first decreased from −1.57 V _SCE to −1.64 V _SCE with an increase in the rotation angle from 0° to 40°, and then increased to −1.60 V _SCE with a further increase in the rotation angle to 90°. The results obtained from potentiostatic tests are also in agreement with the trend in potentiodynamic polarization tests as a function of rotation angle. A similar trend was also observed for the depressed semicircle and the total resistances in the EIS measurements due to the facile formation of MgO and Mg(OH)₂ passive films on the magnesium surface. In addition, the amount of chloride in the passive film was found first to increase with an increase in rotation angle from 0° to 40°, then decrease with a further increase in rotation angle, indicating that the tendency to form a more protective passive film increased for rotation angle near 0° [the (0001) plane] or 90° [the (1010) plane].