Design, construction, and validation of a 1-mm triple-resonance high-temperature-superconducting probe for NMR

We report a 600-MHz 1-mm triple-resonance high-temperature-superconducting (HTS) probe for nuclear magnetic resonance spectroscopy. The probe has a real sample volume of about 7.5 microl, an active volume of 6.3 microl, and appears to have the highest mass sensitivity at any field strength. The probe is constructed with four sets of HTS coils that are tuned to 1H, 2H, 13C, and 15N, and there is a z-axis gradient. The coils are cooled with a conventional Bruker CryoPlatform to about 20 K, and the sample chamber can be regulated above or below room temperature over a moderate range using a Bruker variable temperature unit. The absolute S/N for 0.1% ethylbenzene is approximately 1/3 that of a conventional 5mm probe with just 1/70 of the sample volume. We demonstrate the utility of this probe for small molecules and proteins with 2D spectra of just 1.7 microg of ibuprofen and 400 microM 15N-labeled ubiquitin.     

Study of a Crack at a Fastener Hole by Digital Image Correlation

In this work the efficacy of using digital image correlation to determine stress intensity factors for a crack emanating from a fastener hole has been investigated. To this end a fatigue crack was grown in pure mode I from a 50 mm diameter hole in an Al 7010 alloy plate test-piece. This crack was then loaded elastically under several combinations of mixed mode (I + II) displacements. In each case, images of the sample surface before and after the deformation were recorded using a high resolution digital camera. The surface preparation consisted only of scratching the surface lightly with silicon carbide abrasive paper. The crack location and resulting displacements were then calculated using digital image correlation. The analytical displacement fields for a traction free crack under arbitrary loading conditions based on the Muskhelishvili’s complex function approach were fitted to the experimentally measured displacement fields and the mixed mode stress intensity factor was determined in each case. Good agreement with the nominal applied values was obtained. The uncertainty of the crack tip position has a major influence on the accuracy of the stress intensity factors and so the Sobel edge finding filter was successfully applied to experimental displacement fields to establish precisely the crack tip location. This paper was presented at the 2007 SEM Congress held in Springfield, Massachusetts, USA     

K(0.46)Na(0.54)NbO3 ferroelectric ceramics: chemical synthesis, electro-mechanical characteristics, local crystal chemistry and elastic anomalies

K(0.46)Na(0.54)NbO(3) ceramics have been fabricated via a chemical synthesis route. It was found that 500 °C heat treatment is sufficient to crystallize the niobate powder and the ceramic sintered at 1080 °C in air shows good ferroelectric and piezoelectric properties (P(r) ~ 15 μC cm(-2), d(33) ~ 120 pC N(-1)). Electron diffraction patterns not only determine the space group symmetry of Pcm2(1) for the first time, but also reveal structural disorder in K(0.46)Na(0.54)NbO(3), and 1-D correlated strings of Nb-O atomic displacements are suggested to account for the polar behaviour. Elastic constants such as the bulk and shear moduli as well as their evolution with temperature were also measured using the resonant ultrasound spectroscopy method.     

Predicting the onset of rafting of γ′ precipitates by channel deformation in a Ni superalloy

The growth or shrinkage, normal to {001}, of the interfaces between the γ matrix and cuboidal γ′ precipitates is examined for a Ni-base superalloy, by considering the force acting on the interfaces. The force is produced by the precipitate coherency misfit and the stress produced by plastic deformation in channels of the γ matrix. A simple expression, which directly addresses the origin of the surface force, is given. The plastic deformation within the initially active γ matrix channels exerts the force to cause rafting. The subsequent activation of other types of channels also promotes the rafting in the same direction as the first active channels, when the plastic strain of the former channels increases. These issues are also discussed in terms of analysis based on those dislocations caused by the precipitate misfit and those produced by the plastic deformation.