In-liquid bulk acoustic wave resonators for biosensing applications

Gravimetric sensors based on thin-film bulk acoustic wave (BAW) resonators operating between 1-5 GHz have tremendous potential as biosensors because they are inexpensive, label-free, fast and highly sensitive. The two main challenges in this objective are: the conventional longitudinal mode resonance in $\textit{c}$-axis oriented piezoelectric films suffers from more than 90% damping in liquid; the alternative is the shear mode resonance, with lower damping in liquid but which requires an inclined $\textit{c}$-axis piezoelectric film, a process that is still not fully scalable. In this thesis, seed layers such as AlN with mainly (103) orientations are used to promote the growth of homogeneously inclined $\textit{c}$-axis ZnO (inclination of up to $\sim$45$^{\circ}$) films without significant equipment modifications. Sputtered Al electrodes with controlled roughness are then substituted for the parasitic AlN seed layers to improve the electromechanical performance. At a substrate temperature, T$_{s}$ = 100 $^{\circ}$C, an optimum surface roughness of 9.2 nm yields homogeneously inclined $\textit{c}$-axis ZnO films with angles $\sim$25$^{\circ}$. Solidly mounted resonators (SMRs) operating in a shear mode at $\sim$1.1 GHz with the Al electrodes have resonant quality factors (Q$_{r}$) higher than 150 and effective electromechanical coupling coefficients, k$^{2}$$_{eff}$, of 2.9-3.4%, which are improved from only 2.2% with the AlN seed layers. This shear mode of the ZnO SMRs has mass sensitivities, S$_{m}$ of (4.9 $\pm$ 0:1) kHz$\cdot$cm$^{2}$/ng and temperature coefficients of frequency (TCF) of -(66$\pm$2) ppm/K. Viscosity sensing is carried out with different ethanol-water compositions; the SMRs are functionalised and successfully used in the detection of Rabbit Immunoglobin G. To mitigate the longitudinal mode damping in water, multi-wall carbon nanotube (CNT) forests are grown by chemical vapour deposition (CVD) at 600 $^{\circ}$C using Fe/Al layers on the active area of inclined $\textit{c}$-axis AlN SMRs designed for improved thermal and chemical stability. The dense CNT forest (with 0.5/8 nm Fe/Al) of $\sim$15 μm height provides an acoustic isolation to DI water with only 50-70% drop in the longitudinal mode Q$_{r}$ compared to 99% in SMRs without the CNTs. Mass loading is still detected and demonstrated by detecting bovine serum albumin (BSA) in water whereas with forest heights of $\sim$30 μm and no significant frequency shifts due to mass attachment are observed. With the CNTs the longitudinal mode is shown for the first time to be more sensitive to mass ($\sim$7x) than the shear mode in liquid, highlighting the potential of CNTs for the large scale use of the longitudinal mode for in-liquid sensing

Investigation of flexural plate wave devices for sensing applications in liquid media

In this thesis, the author proposes and presents a novel simulation technique for the analysis of multilayered Flexural Plate Wave (FPW) devices based on the convergence of the Finite Element method (FEM) with classical Surface Acoustic Wave (SAW) analysis techniques and related procedures. Excellent agreement has been obtained between the author's approach and other more conventional modelling techniques. Utilisation of the FEM allows the performance characteristics of a FPW structure to be critically investigated and refined before undertaking the costly task of fabrication. Based on a series of guidelines developed by the author, it is believed the proposed technique can also be applied to other acoustic wave devices. The modelling process developed is quite unique as it is independent of the problem geometry as verified by both two and three dimensional simulations. A critic al review of FEM simulation parameters is presented and their effect on the frequency domain response of a FPW transducer given. The technique is also capable of simultaneously modelling various second-order effects, such as triple transit, diffraction and electromagnetic feedthrough, which often requires the application of several different analysis methodologies. To verify the results obtained by the author's novel approach, several commonly used numerical techniques are discussed and their limitations investigated. The author initially considers the Transmission Matrix method, where it is shown that an inherent numerical instability prevents solution convergence when applied to large frequency-thickness products and complex material properties which are characteristic of liquids. In addition the Stiffness Matrix method is investigated, which is shown to be unconditionally stable. Based on this technique, particle displacement profiles and mass sensitivity are presented for multilayered FPW structures and compared against simpler single layer devices commonly quoted in literature. Significant differences are found in mass sensitivity between single layer and multilayered structures. Frequency response characteristics of a FPW device are then explored via a spectral domain Green's function, which serves as a further verification technique of the author's novel analysi s procedure. Modifications to the spectral domain Green's function are discussed and implemented due to the change in solution geometry from SAW to FPW structures. Using the developed techniques, an analysis is undertaken on the applicability of FPW devices for sensing applications in liquid media. Additions are made to both the Stiffness Matrix method and FEM to allow these techniques to accurately incorporate the influence of a liquid layer. The FEM based approach is then applied to obtain the frequency domain characteristics of a liquid loaded FPW structure, where promising results have been obtained. Displacement profiles are considered in liquid media, where it is shown that a tightly coupled Scholte wave exists that is deemed responsible for most reported liquid sensing results. The author concludes the theoretical analysis with an in-depth analysis of a FPW device when applied to density, viscosity and mass sensing applications in liquid media. It is shown that a single FPW device is potentially capable of discriminating between density and viscosity effects, which is typically a task that requires a complex and costly sensor array

Sonocytology: dynamic acoustic manipulation of particles and cells

Separating and sorting cells and micro-organisms from a heterogeneous mixture is a fundamental step in biological, chemical and clinical studies, enabling regenerative medicine, stem cell research, clinical sample preparation and improved food safety. Particle and cell manipulation by ultrasound acoustic waves provides the capability of separation of cells on the basis of their size and physical properties. Offering the advantages of relatively large microfluidic volumes in a label-free, contactless and biocompatible manner. Consequently, the discovery of alternative methods for precise manipulation of cells and particles is of highly demand. This thesis describes a novel approach of ultrasound acoustic manipulation of particles and cells. The principle of operation of the dynamic acoustic field method is described accompanied with acoustic separation simulations. Furthermore, the complete fabrication and characterisation of two types of ultrasound devices is given. The first one is a bulk acoustic wave (BAW) device and the second is a surface acoustic wave (SAW) device. Successful experiments using the BAW device for sorting different diameter particles with a range from 5 to 45 μm are demonstrated, also experiments for sorting particles depending on their density are presented. Moreover, experiments of the proposed method for sorting porcine dorcal root ganglion (DRG) cells from a heterogeneous mixture of myelin debris depending on their size are displayed. Experimental results of sorting cells depending on their stiffness are demonstrated. Experiments using the fabricated SAW device for sorting different diameter particles in a constant flow with a range from 1 μm to 10 μm are presented. Furthermore, experiments of the proposed method for sorting live from dead Htert cells depending on their mechanical properties, i.e. stiffness are displayed. As a side project a new idea for dynamic acoustic manipulation by rotating the acoustic field is demonstrated. The basic principles of this method and the simulations for verifying this concept are displayed. Experiments for sorting 10 μm from 3 μm polystyrene particles are presented, with two different types of the dynamic acoustic rotating field being examined

Additively manufactured lattice structures for vibration attenuation

Advancements in additive manufacturing technology have allowed the realisation of geometrically complex structures with enhanced capabilities in comparison to solid structures. One of these capabilities is vibration attenuation which is of paramount importance for the precision and accuracy of metrology and machining instruments. In this project, new additively manufactured lattice structures are proposed for achieving vibration attenuation. The ability of these lattices to provide vibration attenuation at frequencies greater than their natural frequency was studied first. This is referred to as vibration isolation. For the vibration isolation study, a combination of finite element modelling and an experimental setup comprising a dynamic shaker and laser vibrometer was used. The natural frequencies obtained from the experimental results were 93 % in agreement with the simulated results. However, vibration attenuation was demonstrated only along one dimension and vibration waves were allowed to propagate, meaning the transmissibility was allowed to be greater than 0 dB. To achieve lower transmissibility, the project demonstrated that lattice structures can develop Bragg-scattering and internal resonance bandgaps. The bandgaps were identified from the lattices' dispersion curves calculated using a finite element based wave propagation modelling technique. Triply periodic minimal surface lattices and strut-based lattices developed Bragg-scattering bandgaps with a normalised bandgap frequency (wavelength divided by cell size) of ~ 0.2. The bandgap of the tested lattices was demonstrated to be tunable with the volume fraction of the lattice unit cell, thus, providing a tool to design lattice structures with bandgaps at required frequencies. An internal resonance mechanism in the form of a solid cube or sphere with struts was designed into the inner core of the unit cell of strut-based lattices. These new internal resonance lattices can provide (a) lower frequency bandgaps than Bragg-scattering lattices within the same design volume, and/or (b) comparable bandgaps frequencies with reduced unit cell dimensions. In comparison to lattices of higher normalised bandgap frequencies, lattices with lower normalised bandgap frequencies have cell sizes that are more suitable for manufacturing with the current additive manufacturing technologies and have higher periodicity within a constrained design volume, resulting in higher attenuation within the bandgaps and more homogenous structures. Similar to the Bragg-scattering lattices, the bandgaps of the internal resonance lattices were demonstrated to be tunable through modification of the geometry of the lattice unit cell. The internal resonance lattice experimentally demonstrated a bandgap of normalised frequency between 0.039 to 0.067 and an attenuation of up to -77 dB. These results are essential for engineering vibration attenuation capabilities within the macro-scale of materials for complete elimination of all mechanical vibration waves at tailorable frequencies. Future work will include further reduction of the bandgap frequencies and increasing the bandgap width by exploring new unit cell designs and new materials for additive manufacturing