Design and construction of an ultrasonic probe for use in a Cryo-Magnet NMR Spectrometer

SINNMR (Sonically Induced Narrowing of the Nuclear Magnetic Resonance spectra of solids), is a novel technique that is being developed to enable the routine study of solids by nuclear magnetic resonance spectroscopy. SINNMR aims to narrow the broad resonances that are characteristic of solid state NMR by inducing rapid incoherent motion of solid particles suspended in a support medium, using high frequency ultrasound in the range 2-10 MHz. The width of the normal broad resonances from solids are due to incomplete averaging of several components of the total spin Hamiltonian caused by restrictions placed on molecular motion within a solid. At present Magic Angle Spinning (MAS) NMR is the classical solid state technique used to reduce line broadening, but: this has associated problems, not least of which is the appearance of many spinning side bands which confuse the spectra. It is hoped that SlNNMR will offer a simple alternative, particularly as it does not reveal spinning sidebands The fundamental question concerning whether the use of ultrasound within a cryo-magnet will cause quenching has been investigated with success, as even under the most extreme conditions of power, frequency and irradiator time, the magnet does not quench. The objective of this work is to design and construct a SINNMR probe for use in a super conducting cryo-magnet NMR spectrometer. A cell for such a probe has been constructed and incorporated into an adapted high resolution broadband probe. It has been proved that the cell is capable of causing cavitation, up to 10 MHz, by running a series of ultrasonic reactions within it and observing the reaction products. It was found that the ultrasound was causing the sample to be heated to unacceptable temperatures and this necessitated the incorporation of temperature stabilisation devices. Work has been performed on the investigation of the narrowing of the solid state 23Na spectrum of tri-sodium phosphate using high frequency ultrasound. Work has also been completed on the signal enhancement and T1 reduction of a liquid mixture and a pure compound using ultrasound. Some preliminary "bench" experiments have been completed on a novel ultrasonic device designed to help minimise sample heating. The concept involves passing the ultrasound through a temperature stabilised, liquid filled funnel that has a drum skin on the end that will enable the passage of ultrasound into the sample. Bench experiments have proved that acoustic attenuation is low and that cavitation in the liquid beyond the device is still possible.

Transducer diffraction theory and development of an ultrasonic tomogram

The work described in this thesis is the development of an ultrasonic tomogram to provide outlines of cross-sections of the ulna in vivo. This instrument, used in conjunction with X-ray densitometry previously developed in this department, would provide actual bone mineral density to a high resolution. It was hoped that the accuracy of the plot obtained from the tomogram would exceed that of existing ultrasonic techniques by about five times. Repeat measurements with these instruments to follow bone mineral changes would involve very low X-ray doses. A theoretical study has been made of acoustic diffraction, using a geometrical transform applicable to the integration of three different Green's functions, for axisymmetric systems. This has involved the derivation of one of these in a form amenable to computation. It is considered that this function fits the boundary conditions occurring in medical ultrasonography more closely than those used previously. A three dimensional plot of the pressure field using this function has been made for a ring transducer, in addition to that for disc transducers using all three functions. It has been shown how the theory may be extended to investigate the nature and magnitude of the particle velocity, at any point in the field, for the three functions mentioned. From this study. a concept of diffraction fronts has been developed, which has made it possible to determine energy flow also in a diffracting system. Intensity has been displayed in a manner similar to that used for pressure. Plots have been made of diffraction fronts and energy flow direction lines.

The mechanics of ultrasonic tube bending

The technology of precision bending of tubes has recently increased in importance and is widely demanded for many industrial applications. However, whilst attention has been concentrated on automation and increasing the production rate of the bending machines, it seems that with one exception very little work has been done in order to understand and therefore fundamentally improve the bending process. A new development for the process of draw-bending of tubes, in which the supporting mandrel is axially vibrated at an ultrasonic frequency, has been perfected. A research programme was undertaken to study the mechanics of tube• bending under both vibratory and non-vibratory conditions. For this purpose, a conventional tube-bending machine was modified and equipped with an oscillatory system. Thin-walled mild steel tubes of different diameter to thickness ratios were bent to mean bend radii having various values from 1.5 to 2.0 times the tube diameter. It was found that the application of ultrasonic vibration reduces the process forces and that the force reduction increases with increasing the vibration amplitude. A reduction in the bending torque of up to 30 per cent was recorded and a reduction in the maximum tube-wall thinning of about 15 per cent was observed. The friction vector reversal mechanism as well as a reduction in friction account for the changes of the forces and the strains. Monitoring the mandrel friction during bending showed, in some cases, that the axial vibration reverses the mandrel .mean force from tension to compression and, thus, the mandrel is assisting the tube motion instead of resisting it. A theory has been proposed to describe the mechanics of deformation during draw-bending of tubes, which embodies the conditions of both "with" and "without" mandrel axial vibration. A theoretical analysis, based on the equilibrium of forces approach, has been developed in which the basic process parameters were taken into consideration. The stresses, the strains and the bending torque were calculated utilising this new solution, and a specially written computer programme was used to perform the computations. It was shown that the theory is in good agreement with the measured values of the strains under vibratory and non-vibratory conditions. Also, the predicted bending 'torque showed a similar trend to that recorded experimentally.

Ultrasonic inspection of austenitic stainless steel weldments

Ultrasonic waves interact in a complex manner with the metallurgical structure of austenitic weldments resulting in ambiguity when interpreting reflections and at times in misinterpretation of defect positions. In this work, current knowledge of the structure of austenitic welds is outlined, and the influence of this structure on the propagation of ultrasonic waves is reviewed. Using an established and highly accurate technique, data on velocity variations as a function of the angle between the direction of soundwave propagation and the axes of preferred grain orientation existing in such welds, are experimentally obtained. These results and existing theory are used to provide quantitative evidence of (i) anisotropy factors in austenitic welds, (ii) beam skewing effects for different wave modes and polarizations, and (iii) the extent of acoustic impedance mismatch between parent and weld metals. The existence of "false" indications is demonstrated, and suggestions are made into their nature. The effectiveness of conventional transverse wave techniques for inspecting artificial and real defects existing in austenitic weldments is experimentally investigated, the limitations are demonstrated, and possible solutions are proposed. The possibilities offered by the use of longitudinal angle probes for ultrasonic inspection of real and artificial defects existing in austenitic weldments are experimentally investigated, and parameters such as probe angle, frequency and scanning position are evaluated. Detailed work has been carried out on the interaction of ultrasound with fatigue and corrosion-fatigue cracks in the weld metal and the heat affected zones (HAZs) of 316 and 347 types of austenitic weldments, together with the influence of elastic compressive stresses, defect topography and defect geometry. Practical applications of all results are discussed, and more effective means of ultrasonic inspection of austenitic weldments are suggested.

Use of ultrasonic agitation in iron group alloy electrodepositions

The effects of ultrasonic agitation on deposition from two iron group alloy plating solutions, nickel-cobalt and bright nickel-iron, have been studied. Comparison has been made with deposits plated from the same solutions using controlled air agitation. The ultrasonic equipment employed had a fixed frequency of 13 KHz but the power output from each transducer was variable up to a maximum of 350 watts. The effects of air and ultrasonic agitation on hardness, ductility, tensile strength, composition, structure, surface topography, limiting current density, cathode current efficiency and macro-throwing power were determined. Transmission and scanning electron microscopy, electron-probe microanalysis and atomic absorption spectrophotometry have been employed to study the nickel alloy deposits produced. The results obtained show that the use of Ultrasonics increased significantly the hardness of both alloy deposits and altered their composition by decreasing the cobalt and iron contents from nickel-cobalt and nickeliron solutions respectively. The ductility of coatings improved but the tensile strength did not change very much. Ultrasonic agitation gave larger grained deposits than air and they seemed to have a lower stress. Dull cobalt-nickel deposits had a similar pyramidal surface topography regardless of the type of agitation but the bright appearance of the nickel-iron was destroyed by ultrasonic agitation; an unusual ribbed pattern was produced. The use of ultrasonic agitation permitted approximately a twofold increase in the plating current density at which sound deposits could be achieved but there was only a slight increase in cathode current efficiency. Macro-throwing power of the solutions was increased slightly by the use of ultrasonic agitation. ultrasonic agitation is an expensive means of agitating plating Solutions and would be worthwhile only if significant improvements in properties could be achieved. The simultaneous improvement in hardness and ductility is a novel feature that should have useful engineering applications.

Embedded fibre Bragg grating array sensors in aluminium alloy matrix by ultrasonic consolidation

Fibre Bragg Grating (FBG) array sensors have been successfully embedded in aluminium alloy matrix by ultrasonic consolidation (UC) technique. The temperature and loading responses of the embedded FBG arrays have been systematically characterised. The embedded grating sensors exhibit an average temperature sensitivity of ~36pm/°C, which is three times higher than that of normal FBGs, and a loading responsivity of ~0.1nm/kg within the dynamic range from 0kg to 3kg. This initial experiment clearly demonstrates that FBG array sensors can be embedded in metal matrix together with other passive and active fibres to fabricate smart materials to monitor the operation and health of engineering structures.

Ultrasonic field and temperature sensor based on short in-fibre Bragg gratings

The authors demonstrate that in-fibre Bragg gratings may be successfully used to measure megahertz acoustic fields if the grating length is sufficiently short and the optical fibre is appropriately desensitised. A noise-limited pressure resolution of 4.5 × 10 –3 atm vHz was found. The capability to simultaneously act as a temperature sensor is also demonstrated.

An energy-efficient route to the rapid synthesis of organically-modified SBA-15 via ultrasonic template removal

A low energy route for the removal of Pluronic P123 surfactant template during the synthesis of SBA-15 mesoporous silicas is explored. The conventional reflux of the hybrid inorganic-organic intermediate formed during co-condensation routes to Pr-SOH-SBA-15 is slow, utilises large solvent volumes, and requires 24 h to remove ∼90% of the organic template. In contrast, room temperature ultrasonication in a small methanol volume achieves the same degree of template extraction in only 5 min, with a 99.9% energy saving and 90% solvent reduction, without compromising the textural, acidic or catalytic properties of the resultant Pr-SOH-SBA-15. © 2014 The Royal Society of Chemistry.

Ultrasonic hydrophone based on short in-fiber Bragg gratings

We investigate the feasibility of using in-fiber Bragg gratings for measuring acoustic fields in the megahertz range. We found that the acoustic coupling from the ultrasonic field to the grating leads to the formation of standing waves in the fiber. Because of these standing waves, the system response is complex and, as we show, the grating does not act as an effective probe. However, significant improvement in its performance can be gained by use of short gratings coupled with an appropriate desensitization of the fiber. A noise-limited pressure resolution of ˜4.5 × 10-3 atm/vHz was found.