Characterization of Amorphous Tantalum Oxide for Insulating Acoustic Mirrors

This work describes the assessment of the acoustic properties of sputtered tantalum oxide films intended as high impedance films for the acoustic isolation of bulk acoustic wave devices operating in the GHz frequency range. The films are grown by sputtering a metallic tantalum target under different oxygen and argon gas mixtures, total pressures, pulsed DC powers and substrate bias. The structural properties of the films are assessed through infrared absorption spectroscopy and X-ray diffraction measurements. Their acoustic impedance is obtained after estimating the mass density by X-ray reflectometry measurements and the longitudinal acoustic velocity by analyzing the longitudinal λ/2 resonance induced in a tantalum oxide film inserted between an acoustic reflector and an AlN-based resonator. A second measurement of the sound velocity is achieved through picosecond acoustic spectroscopy.

Ta2O5/SiO2 insulating acoustic mirrors for AlN-based X-band BAW resonators

This work describes the performance of AlN-based bulk acoustic wave resonators built on top of insulating acoustic reflectors and operating at around 8 GHz. The acoustic reflectors are composed of alternate layers of amorphous Ta2O5and SiO2 deposited at room temperature by pulsed-DC reactive sputtering in Ar/O2 atmospheres. SiO2 layers have a porous structure that provides a low acoustic impedance of only 9.5 MRayl. Ta2O5 films exhibit an acoustic impedance of around 39.5 MRayl that was assessed by the picoseconds acoustic technique These values allow to design acoustic mirrors with transmission coefficients in the centre of the band lower than -40 dB (99.998 % of reflectance) with only seven layers. The resonators were fabricated by depositing a very thin AlN film onto an iridium bottom electrode 180 nm-thick and by using Ir or Mo layers as top electrode. Resonators with effective electromechanical coupling factors of 5.7% and quality factors at the antiresonant frequency around 600 are achieved.

Influence of Crystal Quality on the Excitation and Propagation of Surface and Bulk Acoustic Waves in Polycrystalline AlN Films

We investigate the excitation and propagation of acoustic waves in polycrystalline aluminum nitride films along the directions parallel and normal to the c-axis. Longitudinal and transverse propagations are assessed through the frequency response of surface acoustic wave and bulk acoustic wave devices fabricated on films of different crystal qualities. The crystalline properties significantly affect the electromechanical coupling factors and acoustic properties of the piezoelectric layers. The presence of misoriented grains produces an overall decrease of the piezoelectric activity, degrading more severely the excitation and propagation of waves traveling transversally to the c-axis. It is suggested that the presence of such crystalline defects in c-axis-oriented films reduces the mechanical coherence between grains and hinders the transverse deformation of the film when the electric field is applied parallel to the surface.

Coupling light into graphene plasmons with the help of surface acoustic waves

We propose a scheme for coupling laser light into graphene plasmons with the help of electrically generated surface acoustic waves. The surface acoustic wave forms a diffraction grating which allows us to excite the long lived phononlike branch of the hybridized graphene plasmon-phonon dispersion with infrared laser light. Our approach avoids patterning the graphene sheet, does not rely on complicated optical near-field techniques, and allows us to electrically switch the coupling between far-field radiation and propagating graphene plasmons.

Fabrication of sub-100 nm IDT SAW devices on insulating, semiconducting and conductive substrates

This work describes the electron-beam (e-beam) lithography process developed to manufacture nano interdigital transducers (IDTs) to be used in high frequency (GHz) surface acoustic wave (SAW) applications. The combination of electron-beam (e-beam) lithography and lift-off process is shown to be effective in fabricating well-defined IDT finger patterns with a line width below 100 nm with a good yield. Working with insulating piezoelectric substrates brings about e-beam deflection. It is also shown how a very thin organic anti-static layer works well in avoiding this charge accumulation during e-beam lithography on the resist layer. However, the use of this anti-static layer is not required with the insulating piezoelectric layer laying on a semiconducting substrate such as highly doped silicon. The effect of the e-beam dose on a number of different layers (of insulating, insulating on semiconducting, semiconducting, and conductive natures) is provided. Among other advantages, the use of reduced e-beam doses increases the manufacturing time. The principal aim of this work is to explain the interrelation among e-beam dose, substrate nature and IDT structure. An extensive study of the e-beam lithography of long IDT-fingers is provided, in a wide variety of electrode widths, electrode numbers and electrode pitches. It is worthy to highlight that this work shows the influence of the e-beam dose on five substrates of different conductive nature

Amorphous piezoresistive and piezoelectric sensors for robotics applications

Ultrasonic transducers have often been used in the development of sensory systems for robotics applications. In most cases, these sensory systems are based on the determination of times of flight for signals from every transducer. In this work we have used piezoresistive and piezoelectric materials to measure the instant and position collision in metallic structures by using the difference of the times of propagation of an acoustic wave when it is produced over a ferromagnetic (iron, steel or another material) based structure. An immediate application of the proposed method is the detection and location of impacts over the metallic links of an industrial robot or the collision position in a metallic structure for an automated inspection

Multiple Frequency Solidly Mounted BAW Filters

This paper reports the simultaneous fabrication of Receive and Transmit Bulk Acoustic Wave filters for the WCDMA standard on the same die. Both filters are based on Solidly Mounted Resonators using a common Bragg mirror, but with each having a specific piezoelectric film thickness. Electrical measurements reveal that the process steps required to provide the two different piezoelectric film thicknesses on the same die does not impact the electrical performances of resonators and filters and that this approach could thus be generalised to more than two filters.

Ultra high frequency thin film saw devices

Durante los últimos años el flujo de datos en la transmisión que tiene lugar en los sistemas de comunicación ha aumentado considerablemente de forma que día a día se requieren más aplicaciones trabajando en un rango de frecuencias muy alto (3-30 GHz). Muchos de estos sistemas de comunicación incluyen dispositivos de onda acústica superficial (SAW) y por tanto se hace necesario el aumento de frecuencia a la que éstos trabajan. Pero este incremento de frecuencia de los dispositivos SAW no sólo es utilizado en los sistemas de comunicación, varios tipos de sensores, por ejemplo, aumentan su sensibilidad cuando la frecuencia a la que trabajan también lo hace. Tradicionalmente los dispositivos SAW se han fabricado sobre cuarzo, LiNbO3 y LiTaO3 principalmente. Sin embargo la principal limitación de estos materiales es su velocidad SAW. Además, debido a la alta temperatura a la que se depositan no pueden ser integrados en la tecnología de fabricación CMOS. El uso de la tecnología de capa delgada, en la que un material piezoeléctrico es depositado sobre un substrato, se está utilizando en las últimas décadas para incrementar la velocidad SAW de la estructura y poder obtener dispositivos trabajando en el rango de frecuencias requerido en la actualidad. Por otra parte, esta tecnología podría ser integrada en el proceso de fabricación CMOS. Durante esta tesis nos hemos centrado en la fabricación de dispositivos SAW trabajando a muy alta frecuencia. Para ello, utilizando la tecnología de capa delgada, hemos utilizado la estructura nitruro de aluminio (AlN) sobre diamante que permite conseguir velocidades SAW del sustrato que no se pueden alcanzar con otros materiales. El depósito de AlN se realizó mediante sputtering reactivo. Durante esta tesis se han realizado diferentes experimentos para optimizar dicho depósito de forma que se han obtenido los parámetros óptimos para los cuales se pueden obtener capas de AlN de alta calidad sobre cualquier tipo de sustrato. Además todo el proceso se realizó a baja temperatura para que el procesado de estos dispositivos pueda ser compatible con la tecnología CMOS. Una vez optimizada la estructura AlN/diamante, mediante litografía por haz de electrones se fabricaron resonadores SAW de tamaño nanométrico que sumado a la alta velocidad resultante de la combinación AlN/diamante nos ha permitido obtener dispositivos trabajando en el rango de 10-28 GHz con un alto factor de calidad y rechazo fuera de la banda. Estás frecuencias y prestaciones no han sido alcanzadas por el momento en resonadores de este tipo. Por otra parte, se han utilizado estos dispositivos para fabricar sensores de presión de alta sensibilidad. Estos dispositivos son afectados altamente por los cambios de temperatura. Se realizó también un exhaustivo estudio de cómo se comportan en temperatura estos resonadores, entre -250ºC y 250ºC (rango de temperaturas no estudiado hasta el momento) diferenciándose dos regiones una a muy baja temperatura en la que el dispositivo muestra un coeficiente de retraso en frecuencia (TCF) relativamente bajo y otra a partir de los -100ºC en la que el TCF es similar al observado en la bibliografía. Por tanto, durante esta tesis se ha optimizado el depósito de AlN sobre diamante para que sea compatible con la tecnología CMOS y permita el procesado de dispositivos trabajando a muy alta frecuencia con altas prestaciones para comunicaciones y sensores. ABSTRACT The increasing volume of information in data transmission systems results in a growing demand of applications working in the super-high-frequency band (3–30 GHz). Most of these systems work with surface acoustic wave (SAW) devices and thus there is a necessity of increasing their resonance frequency. Moreover, sensor application includes this kind of devices. The sensitivity of them is proportional with its frequency. Traditionally, quartz, LiNbO3 and LiTaO3 have been used in the fabrication of SAW devices. These materials suffer from a variety of limitations and in particular they have low SAW velocity as well as being incompatible with the CMOS technology. In order to overcome these problems, thin film technology, where a piezoelectric material is deposited on top of a substrate, has been used during the last decades. The piezoelectric/substrate structure allows to reach the frequencies required nowadays and could be compatible with the mass electronic production CMOS technology. This thesis work focuses on the fabrication of SAW devices working in the super-high-frequency range. Thin film technology has been used in order to get it, especially aluminum nitride (AlN) deposited by reactive sputtering on diamond has been used to increase the SAW velocity. Different experiments were carried out to optimize the parameters for the deposit of high quality AlN on any kind of substrates. In addition, the system was optimized under low temperature and thus this process is CMOS compatible. Once the AlN/diamond was optimized, thanks to the used e-beam lithography, nanometric SAW resonators were fabricated. The combination of the structure and the size of the devices allow the fabrication of devices working in the range of 10-28 GHz with a high quality factor and out of band rejection. These high performances and frequencies have not been reached so far for this kind of devices. Moreover, these devices have been used as high sensitivity pressure sensors. They are affected by temperature changes and thus a wide temperature range (-250ºC to 250ºC) study was done. From this study two regions were observed. At very low temperature, the temperature coefficient of frequency (TCF) is low. From -100ºC upwards the TCF is similar to the one appearing in the literature. Therefore, during this thesis work, the sputtering of AlN on diamond substrates was optimized for the CMOS compatible fabrication of high frequency and high performance SAW devices for communication and sensor application.

High precision pressure sensors based on SAW devices in the GHz range

In this paper, an AlN/free-standing nanocrystalline diamond (NCD) system is proposed in order to process high frequency surface acoustic wave (SAW) resonators for sensing applications. The main problem of synthetic diamond is its high surface roughness that worsens the sputtered AlN quality and hence the device response. In order to study the feasibility of this structure, AlN films from 150 nm up to 1200 nm thick have been deposited on free-standing NCD. We have then analysed the influence of the AlN layer thickness on its crystal quality and device response. Optimized thin films of 300 nm have been used to fabricate of one-port SAW resonators operating in the 10–14 GHz frequency range. A SAW based sensor pressure with a sensibility of 0.33 MHz/bar has been fabricated.

Optimization of AlN thin layers on diamond substrates for high frequency SAW resonators

AlN/diamond heterostructures are very promising for high frequency surface acoustic wave (SAW) resonators. In their design, the thickness of the piezoelectric film is one of the key parameters. On the other hand, the film material quality and, hence, the device performance, also depend on that thickness. In this work, polished microcrystalline diamond substrates have been used to deposit AlN films by reactive sputtering, from 150 nm up to 3 μm thick. A high degree of the c-axis orientation has been obtained in all cases. SAW one port resonators at high frequency have been fabricated on these films with a proper combination of the film thickness and transducer size.

Super-high-frequency SAW resonators on AlN/Diamond

This letter describes the procedure to manufacture high-performance surface acoustic wave (SAW) resonators on AlN/diamond heterostructures working at frequencies beyond 10 GHz. In the design of SAW devices on AlN/diamond systems, the thickness of the piezoelectric layer is a key parameter. The influence of the film thickness on the SAW device response has been studied. Optimized thin films combined with advanced e-beam lithographic techniques have allowed the fabrication of one-port SAW resonators with finger width and pitch of 200 nm operating in the 10–14 GHz range with up to 36 dB out-of-band rejection.

High sensitivity biosensors based on shear mode AIN resonators for in liquid operation

El diagnóstico y detección temprana de enfermedades son clave para reducir la tasa de mortalidad, las hospitalizaciones de larga duración y el desaprovechamiento de recursos. En los últimos años se ha impulsado, mediante un aumento de la financiación, el desarrollo de nuevos biosensores de bajo coste capaces de detectar y cuantificar cantidades muy pequeñas de especies biológicas de una forma barata y sencilla. El trabajo presentado en esta Tesis Doctoral describe la investigación llevada a cabo en el desarrollo de sensores gravimétricos basados en resonadores de ondas acústicas de volumen (BAW) de estructura maciza (SMR). Los dispositivos emplean películas delgadas de A1N como material piezoeléctrico y operan en modo de cizalladura, para así poder detectar especies biológicas en medio líquido. El principio de funcionamiento de estos sensores se basa en la variación que experimenta la frecuencia de resonancia al quedar una pequeña masa adherida a su superficie. Necesitan operar en modo de cizalladura para que su resonancia no se atenúe al trabajar en medio líquido, así como ofrecer una superficie capaz de ser funcionalizada específicamente para la especie biológica a detectar. El reto planteado en esta tesis requiere un acercamiento pluridisciplinar al problema que incluye el estudio de los diferentes materiales que constituyen la estructura multicapa que forma un SMR, el diseño y fabricación del dispositivo y del sistema de fluídica, la funcionalización bioquímica de la superficie del sensor, la demostración de la capacidad de detección de especies biológicas y finalmente el diseño y fabricación de la electrónica asociada para la detección de la señal eléctrica. Todas esas tareas han sido abordadas en las distintas etapas del desarrollo de esta tesis y las contribuciones más relevantes se describen en el documento. En el campo de desarrollo de los materiales, se propone un proceso en dos etapas para la pulverización reactiva de capas de A1N que contengan microcristales inclinados capaces de excitar el modo de cizalladura. Se caracteriza la velocidad acústica del modo de cizalladura en todos los materiales que componen la estructura, con el fin de poder obtener un diseño más adecuado del reflector acústico. Se propone un nuevo tipo de material aislante de alta impedancia acústica consistente en capas de W03 pulverizadas que presenta ciertas ventajas tecnológicas frente a las capas convencionales de Ta205. Respecto del diseño del transductor, se estudia la influencia que tienen los con tactos eléctricos extendidos del resonador necesarios para poder adaptar el sistema de fluídica a la estructura. Los resultados indican que es necesario trabajar sobre sustratos aislantes (tanto el soporte como el espejo acústico) para evitar efectos parásitos asociados al uso de capas metálicas bajo los electrodos del resonador que dañan su resonancia. Se analiza la influencia de las diferentes capas del dispositivo en el coeficiente de temperatura de la frecuencia (TCF) del resonador llegando a la conclusión de que las dos últimas capas del reflector acústico afectan significativamente al TCF del SMR, pudiendo reducirse ajusfando adecuadamente sus espesores. De acuerdo con los resultados de estos estudios, se han diseñado finalmente resonadores SMR operando a f .3 GHz en modo de cizalladura, con un área activa de 65000 /xm2, contactos eléctricos que se extienden f .7 mm y factores de calidad en líquido de f 50. Las extensiones eléctricas permiten adaptar el resonador a un sistema de fluídica de metacrilato. Para la detección de especies biológicas se realiza un montaje experimental que permite circular 800 ¡A por la superficie del sensor a través de un circuito cerrado que trabaja a volumen constante. La circulación de soluciones iónicas sobre el sensor descubierto pone de manifiesto que las altas frecuencias de operación previenen los cortocircuitos y por tanto el aislamiento de los electrodos es prescindible. Se desarrolla un protocolo ad-hoc de funcionalización basado en el proceso estándar APTESGlutaraldehído. Se proponen dos alternativas novedosas para la funcionalización de las áreas activas del sensor basadas en el uso de capas de oxidación de Ir02 y su activación a través de un plasma de oxígeno que no daña al dispositivo. Ambos procesos contribuyen a simplificar notablemente la funcionalización de los sensores gravimétricos. Se utilizan anticuerpos y aptámeros como receptores para detectar trombina, anticuerpo monoclonal IgG de ratón y bacteria sonicadas. Una calibración preliminar del sensor con depósitos de capas finas de Si02 de densidad y espesor conocidos permite obtener una sensibilidad de 1800 kHz/pg-cm2 y un límite de detección of 4.2 pg. Finalmente se propone el prototipo de un circuito electrónico de excitación y lectura de bajo coste diseñado empleando teoría de circuitos de microondas. Aunque su diseño y funcionamiento admite mejoras, constituye la última etapa de un sistema completo de bajo coste para el diagnóstico de especies biológicas basado en resonadores SMR de A1N. ABSTRACT Early diagnosis and detection of diseases are essential for reducing mortality rate and preventing long-term hospitalization and waste of resources. These requirements have boosted the efforts and funding on the research of accurate and reliable means for detection and quantification of biological species, also known as biosensors. The work presented in this thesis describes the development and fabrication of gravimetric biosensors based on piezoelectric AlN bulk acoustic wave (BAW) solidly mounted resonators (SMRs) for detection of biological species in liquid media. These type of devices base their sensing principles in the variation that their resonant frequency suffers when a mass is attached to their surface. They need to operate in the shear mode to maintain a strong resonance in liquid and an adequate functionalisation of their sensing area to guarantee that only the targeted molecules cause the shift. The challenges that need to be overcome to achieve piezoelectric BAW resonators for high sensitivity detection in fluids require a multidisciplinary approach, that include the study of the materials involved, the design of the device and the fluidic system, the biochemical functionalisation of the active area, the experimental proof-of-concept with different target species and the design of an electronic readout circuit. All this tasks have been tackled at different stages of the thesis and the relevant contributions are described in the document. In the field of materials, a two-stage sputtering deposition process has been developed to obtain good-quality AlN films with uniformly tilted grains required to excite the shear mode. The shear acoustic velocities of the materials composing the acoustic reflector have been accurately studied to ensure an optimum design of the reflector stack. WO3 sputtered films have been proposed as high acoustic impedance material for insulating acoustic reflectors. They display several technological advantages for the processing of the resonators. Regarding the design, a study of the influence of the electrical extensions necessary to fit a fluidic system on the performance of the devices has been performed. The results indicate that high resistivity substrates and insulating reflectors are necessary to avoid the hindering of the resonance due to the parasitic effects induced by the extensions. The influence of the different layers of the stack on the resultant TCF of the SMRs has also been investigated. The two layers of the reflector closer to the piezoelectric layer have a significant influence on the TCF, which can be reduced by modifying their thicknesses accordingly. The data provided by these studies has led to the final design of the devices, which operate at 1.3 GHz in the shear mode and display an active area of 65000 /xm2 and electrical extensions of 1.7 mm while keeping a Qahear=150 in liquid. The extensions enable to fit a custom-made fluidic system made of methacrylate. To perform the biosensing experiments, an experimental setup with a liquid closed circuit operating at constant flow has been developed. Buffers of ionic characteristics have been tested on non-isolated devices, revealing that high operation frequencies prevent the risk of short circuit. An ad-hoc functionalisation protocol based on the standard APTES - Glutaraldehyde process has been developed. It includes two new processes that simplify the fabrication of the transducers: the use of IrO2 as oxidation layer and its functionalisation through an O2 plasma treatment that does not damage the resonators. Both antibodies and aptamers are used as receptors. In liquid sensing proof-of-concept experiments with thrombin, IgG mouse monoclonal antibody and sonicated bacteria have been displayed. A preliminary calibration of the devices using SiO2 layers reveals a sensitivity of 1800 kHz/pg-cm2 and a limit of detection of 4.2 pg. Finally, a first prototype of a low-cost electronic readout circuit designed using a standard microwave approach has been developed. Although its performance can be significantly improved, it is an effective first approach to the final stage of a portable low-cost diagnostic system based on shear mode AlN SMRs.

In situ acoustic methods to estimate the physical and mechanical aging of oriented strand board

Following the success achieved in previous research projects usin non-destructive methods to estimate the physical and mechanical aging of particle and fibre boards, this paper studies the relationships between aging, physical and mechanical changes, using non-destructive measurements of oriented strand board (OSB). 184 pieces of OSB board from a French source were tested to analyze its actual physical and mechanical properties. The same properties were estimated using acoustic non-destructive methods (ultrasound and stress wave velocity) during a physical laboratory aging test. Measurements were recorded of propagation wave velocity with the sensors aligned, edge to edge, and forming an angle of 45 degrees, with both sensors on the same face of the board. This is because aligned measures are not possible on site. The velocity results are always higher in 45 degree measurements. Given the results of statistical analysis, it can be concluded that there is a strong relationship between acoustic measurements and the decline in physical and mechanical properties of the panels due to aging. The authors propose several models to estimate the physical and mechanical properties of board, as well as their degree of aging. The best results are obtained using ultrasound, although the difference in comparison with the stress wave method is not very significant. A reliable prediction of the degree of deterioration (aging) of board is presented.

Super-resolution for a point source using positive refraction

Leonhardt demonstrated (2009) that the 2D Maxwell Fish Eye lens (MFE) can focus perfectly 2D Helmholtz waves of arbitrary frequency, i.e., it can transport perfectly an outward (monopole) 2D Helmholtz wave field, generated by a point source, towards a receptor called "perfect drain" (PD) located at the corresponding MFE image point. The PD has the property of absorbing the complete radiation without radiation or scattering and it has been claimed as necessary to obtain super-resolution (SR) in the MFE. However, a prototype using a "drain" different from the PD has shown λ/5 resolution for microwave frequencies (Ma et al, 2010). Recently, the SR properties of a device equivalent to the MFE, called the Spherical Geodesic Waveguide (SGW) (Miñano et al, 2012) have been analyzed. The reported results show resolution up to λ /3000, for the SGW loaded with the perfect drain, and up to λ /500 f for the SGW without perfect drain. The perfect drain was realized as a coaxial probe loaded with properly calculated impedance. The SGW provides SR only in a narrow band of frequencies close to the resonance Schumann frequencies. Here we analyze the SGW loaded with a small "perfect drain region" (González et al, 2011). This drain is designed as a region made of a material with complex permittivity. The comparative results show that there is no significant difference in the SR properties for both perfect drain designs.

Perfect imaging of point sources with positive refraction

The capability of a device called the Spherical Geodesic Waveguide (SGW) to produce images with details below the classic Abbe diffraction limit (super-resolution) is analyzed here. The SGW is an optical system equivalent (by means of Transformation Optics) to the Maxwell Fish Eye (MFE) refractive index distribution. Recently, it has been claimed that the necessary condition to get super-resolution in the MFE and the SGW is the use of a Perfect Point Drain (PPD). The PPD is a punctual receptor placed in the focal point that absorbs the incident wave, without reflection or scattering. A microwave circuit comprising three elements, the SGW, the source and the drain (two coaxial lines loaded with specific impedances) is designed and simulated in COMSOL. The super-resolution properties have been analyzed for different position of the source and drain and for two different load impedances: the PPD and the characteristic line impedance. The results show that in both cases super-resolution occurs only for discrete number of frequencies. Out of these frequencies, the SGW does not show SR in the analysis carried out.