CMOS integration of AlN based piezoelectric microcantilevers

El gran crecimiento de los sistemas MEMS (Micro Electro Mechanical Systems) así como su presencia en la mayoría de los dispositivos que usamos diariamente despertó nuestro interés. Paralelamente, la tecnología CMOS (Complementary Metal Oxide Semiconductor) es la tecnología más utilizada para la fabricación de circuitos integrados. Además de ventajas relacionadas con el funcionamiento electrónico del dispositivo final, la integración de sistemas MEMS en la tecnología CMOS reduce significantemente los costes de fabricación. Algunos de los dispositivos MEMS con mayor variedad de aplicaciones son los microflejes. Estos dispositivos pueden ser utilizados para la extracción de energía, en microscopios de fuerza atómica o en sensores, como por ejemplo, para biodetección. Los materiales piezoeléctricos más comúnmente utilizados en aplicaciones MEMS se sintetizan a altas temperaturas y por lo tanto no son compatibles con la tecnología CMOS. En nuestro caso hemos usado nitruro de alumino (AlN), que se deposita a temperatura ambiente y es compatible con la tecnología CMOS. Además, es biocompatible, y por tanto podría formar parte de un dispositivo que actúe como biosensor. A lo largo de esta tesis hemos prestado especial atención en desarrollar un proceso de fabricación rápido, reproducible y de bajo coste. Para ello, todos los pasos de fabricación han sido minuciosamente optimizados. Los parámetros de sputtering para depositar el AlN, las distintas técnicas y recetas de ataque, los materiales que actúan como electrodos o las capas sacrificiales para liberar los flejes son algunos de los factores clave estudiados en este trabajo. Una vez que la fabricación de los microflejes de AlN ha sido optimizada, fueron medidos para caracterizar sus propiedades piezoeléctricas y finalmente verificar positivamente su viabilidad como dispositivos piezoeléctricos. ABSTRACT The huge growth of MEMS (Micro Electro Mechanical Systems) as well as their presence in most of our daily used devices aroused our interest on them. At the same time, CMOS (Complementary Metal Oxide Semiconductor) technology is the most popular technology for integrated circuits. In addition to advantages related with the electronics operation of the final device, the integration of MEMS with CMOS technology reduces the manufacturing costs significantly. Some of the MEMS devices with a wider variety of applications are the microcantilevers. These devices can be used for energy harvesting, in an atomic force microscopes or as sensors, as for example, for biodetection. Most of the piezoelectric materials used for these MEMS applications are synthesized at high temperature and consequently are not compatible with CMOS technology. In our case we have used aluminum nitride (AlN), which is deposited at room temperature and hence fully compatible with CMOS technology. Otherwise, it is biocompatible and and can be used to compose a biosensing device. During this thesis work we have specially focused our attention in developing a high throughput, reproducible and low cost fabrication process. All the manufacturing process steps of have been thoroughly optimized in order to achieve this goal. Sputtering parameters to synthesize AlN, different techniques and etching recipes, electrode material and sacrificial layers are some of the key factors studied in this work to develop the manufacturing process. Once the AlN microcantilevers fabrication was optimized, they were measured to characterize their piezoelectric properties and to successfully check their viability as piezoelectric devices.

Design, Technology and Characterization of Micromechanised Sensors and Actuators for Harsh Environments

Los sistemas micro electro mecánicos (MEMS) han demostrado ser una exitosa familia de dispositivos que pueden usarse como plataforma para el desarrollo de dispositivos con aplicaciones en óptica, comunicaciones, procesado de señal y sensorización. Los dispositivos MEMS estándar suelen estar fabricados usando tecnología de silicio. Sin embargo, el rendimiento de estos MEMS se puede mejorar si se usan otros materiales. Por ejemplo, el diamante nanocristalino (NCD) ofrece unas excelentes propiedades mecánicas, transparencia y una superficie fácil de funcionalizar. Por otro lado, el sistema de materiales (In; Ga; Al)N, los materiales IIIN, se pueden usar para producir estructuras monocristalinas con alta sensibilidad mecánica y química. Además, el AlN se puede depositar por pulverización catódica reactiva sobre varios substratos, incluyendo NCD, para formar capas policristalinas orientadas con alta respuesta piezoeléctrica. Adicionalmente, tanto el NCD como los materiales III-N muestran una gran estabilidad térmica y química, lo que los hace una elección idónea para desarrollar dispositivos para aplicaciones para alta temperatura, ambientes agresivos e incluso para aplicaciones biocompatibles. En esta tesis se han usado estos materiales para el diseño y medición de demostradores tecnológicos. Se han perseguido tres objetivos principales: _ Desarrollo de unos procesos de fabricación apropiados. _ Medición de las propiedades mecánicas de los materiales y de los factores que limitan el rendimiento de los dispositivos. _ Usar los datos medidos para desarrollar dispositivos demostradores complejos. En la primera parte de esta tesis se han estudiado varias técnicas de fabricación. La estabilidad de estos materiales impide el ataque y dificulta la producción de estructuras suspendidas. Los primeros capítulos de esta disertación se dedican al desarrollo de unos procesos de transferencia de patrones por ataque seco y a la optimización del ataque húmedo sacrificial de varios substratos propuestos. Los resultados de los procedimientos de ataque se presentan y se describe la optimización de las técnicas para la fabricación de estructuras suspendidas de NCD y materiales III-N. En un capítulo posterior se estudia el crecimiento de AlN por pulverización catódica. Como se ha calculado en esta disertación para obtener una actuación eficiente de MEMS, las capas de AlN han de ser finas, típicamente d < 200 nm, lo que supone serias dificultades para la obtención de capas orientadas con respuesta piezoeléctrica. Las condiciones de depósito se han mapeado para identificar las fronteras que proporcionan el crecimiento de material orientado desde los primeros pasos del proceso. Además, durante la optimización de los procesos de ataque se estudió un procedimiento para fabricar películas de GaN nanoporoso. Estas capas porosas pueden servir como capas sacrificiales para la fabricación de estructuras suspendidas de GaN con baja tensión residual o como capas para mejorar la funcionalización superficial de sensores químicos o biológicos. El proceso de inducción de poros se discutirá y también se presentarán experimentos de ataque y funcionalización. En segundo lugar, se han determinado las propiedades mecánicas del NCD y de los materiales III-N. Se han fabricado varias estructuras suspendidas para la medición del módulo de Young y de la tensión residual. Además, las estructuras de NCD se midieron en resonancia para calcular el rendimiento de los dispositivos en términos de frecuencia y factor de calidad. Se identificaron los factores intrínsecos y extrínsecos que limitan ambas figuras de mérito y se han desarrollado modelos para considerar estas imperfecciones en las etapas de diseño de los dispositivos. Por otra parte, los materiales III-N normalmente presentan grandes gradientes de deformación residual que causan la deformación de las estructuras al ser liberadas. Se han medido y modelado estos efectos para los tres materiales binarios del sistema para proporcionar puntos de interpolación que permitan predecir las características de las aleaciones del sistema III-N. Por último, los datos recabados se han usado para desarrollar modelos analíticos y numéricos para el diseño de varios dispositivos. Se han estudiado las propiedades de transducción y se proporcionan topologías optimizadas. En el último capítulo de esta disertación se presentan diseños optimizados de los siguientes dispositivos: _ Traviesas y voladizos de AlN=NCD con actuación piezoeléctrica aplicados a nanoconmutadores de RF para señales de alta potencia. _ Membranas circulares de AlN=NCD con actuación piezoeléctrica aplicadas a lentes sintonizables. _ Filtros ópticos Fabry-Pérot basados en cavidades aéreas y membranas de GaN actuadas electrostáticamente. En resumen, se han desarrollado unos nuevos procedimientos optimizados para la fabricación de estructuras de NCD y materiales III-N. Estas técnicas se han usado para producir estructuras que llevaron a la determinación de las principales propiedades mecánicas y de los parámetros de los dispositivos necesarios para el diseño de MEMS. Finalmente, los datos obtenidos se han usado para el diseño optimizado de varios dispositivos demostradores. ABSTRACT Micro Electro Mechanical Systems (MEMS) have proven to be a successful family of devices that can be used as a platform for the development of devices with applications in optics, communications, signal processing and sensorics. Standard MEMS devices are usually fabricated using silicon based materials. However, the performance of these MEMS can be improved if other material systems are used. For instance, nanocrystalline diamond (NCD) offers excellent mechanical properties, optical transparency and ease of surface functionalization. On the other hand, the (In; Ga; Al)N material system, the III-N materials, can be used to produce single crystal structures with high mechanical and chemical sensitivity. Also, AlN can be deposited by reactive sputtering on various substrates, including NCD, to form oriented polycrystalline layers with high piezoelectric response. In addition, both NCD and III-N materials exhibit high thermal and chemical stability, which makes these material the perfect choice for the development of devices for high temperatures, harsh environments and even biocompatible applications. In this thesis these materials have been used for the design and measurement of technological demonstrators. Three main objectives have been pursued: _ Development of suitable fabrication processes. _ Measurement of the material mechanical properties and device performance limiting factors. _ Use the gathered data to design complex demonstrator devices. In a first part of the thesis several fabrication processes have been addressed. The stability of these materials hinders the etching of the layers and hampers the production of free standing structures. The first chapters of this dissertation are devoted to the development of a dry patterning etching process and to sacrificial etching optimization of several proposed substrates. The results of the etching processes are presented and the optimization of the technique for the manufacturing of NCD and III-N free standing structures is described. In a later chapter, sputtering growth of thin AlN layers is studied. As calculated in this dissertation, for efficient MEMS piezoelectric actuation the AlN layers have to be very thin, typically d < 200 nm, which poses serious difficulties to the production of c-axis oriented material with piezoelectric response. The deposition conditions have been mapped in order to identify the boundaries that give rise to the growth of c-axis oriented material from the first deposition stages. Additionally, during the etching optimization a procedure for fabricating nanoporous GaN layers was also studied. Such porous layers can serve as a sacrificial layer for the release of low stressed GaN devices or as a functionalization enhancement layer for chemical and biological sensors. The pore induction process will be discussed and etching and functionalization trials are presented. Secondly, the mechanical properties of NCD and III-N materials have been determined. Several free standing structures were fabricated for the measurement of the material Young’s modulus and residual stress. In addition, NCD structures were measured under resonance in order to calculate the device performance in terms of frequency and quality factor. Intrinsic and extrinsic limiting factors for both figures were identified and models have been developed in order to take into account these imperfections in the device design stages. On the other hand, III-N materials usually present large strain gradients that lead to device deformation after release. These effects have been measured and modeled for the three binary materials of the system in order to provide the interpolation points for predicting the behavior of the III-N alloys. Finally, the gathered data has been used for developing analytic and numeric models for the design of various devices. The transduction properties are studied and optimized topologies are provided. Optimized design of the following devices is presented at the last chapter of this dissertation: _ AlN=NCD piezoelectrically actuated beams applied to RF nanoswitches for large power signals. _ AlN=NCD piezoelectrically actuated circular membranes applied to tunable lenses. _ GaN based air gap tunable optical Fabry-Pérot filters with electrostatic actuation. On the whole, new optimized fabrication processes has been developed for the fabrication of NCD and III-N MEMS structures. These processing techniques was used to produce structures that led to the determination of the main mechanical properties and device parameters needed for MEMS design. Lastly, the gathered data was used for the design of various optimized demonstrator devices.

Piezoelectric sensing and non-parametric statistical signal processing for health monitoring of hysteretic dampers used in seismic-resistant structures

The paper proposes a new application of non-parametric statistical processing of signals recorded from vibration tests for damage detection and evaluation on I-section steel segments. The steel segments investigated constitute the energy dissipating part of a new type of hysteretic damper that is used for passive control of buildings and civil engineering structures subjected to earthquake-type dynamic loadings. Two I-section steel segments with different levels of damage were instrumented with piezoceramic sensors and subjected to controlled white noise random vibrations. The signals recorded during the tests were processed using two non-parametric methods (the power spectral density method and the frequency response function method) that had never previously been applied to hysteretic dampers. The appropriateness of these methods for quantifying the level of damage on the I-shape steel segments is validated experimentally. Based on the results of the random vibrations, the paper proposes a new index that predicts the level of damage and the proximity of failure of the hysteretic damper

Piezoelectric polymer transducers for dynamic pressure measurements. Final report.

National Highway Traffic Safety Administration, Washington, D.C.

Modelling the input-output behaviour of piezoelectric structural health monitoring systems for composite plates

This paper investigates the input-output characteristics of structural health monitoring systems for composite plates based on permanently attached piezoelectric transmitter and sensor elements. Using dynamic piezoelectricity theory and a multiple integral transform method to describe the propagating and scattered flexural waves an electro-mechanical model for simulating the voltage input-output transfer function for circular piezoelectric transmitters and sensors adhesively attached to an orthotropic composite plate is developed. The method enables the characterization of all three physical processes, i.e. wave generation, wave propagation and wave reception. The influence of transducer, plate and attached electrical circuit characteristics on the voltage output behaviour of the system is examined through numerical calculations, both in frequency and the time domain. The results show that the input-output behaviour of the system is not properly predicted by the transducers' properties alone. Coupling effects between the transducers and the tested structure have to be taken into account, and adding backing materials to the piezoelectric elements can significantly improve the sensitivity of the system. It is shown that in order to achieve maximum sensitivity, particular piezoelectric transmitters and sensors need to be designed according to the structure to be monitored and the specific frequency regime of interest.

Non-linear analysis of the thermo-electro-mechanical behaviour of shear deformable FGM plates with piezoelectric actuators

This paper investigates the non-linear bending behaviour of functionally graded plates that are bonded with piezoelectric actuator layers and subjected to transverse loads and a temperature gradient based on Reddy's higher-order shear deformation plate theory. The von Karman-type geometric non-linearity, piezoelectric and thermal effects are included in mathematical formulations. The temperature change is due to a steady-state heat conduction through the plate thickness. The material properties are assumed to be graded in the thickness direction according to a power-law distribution in terms of the volume fractions of the constituents. The plate is clamped at two opposite edges, while the remaining edges can be free, simply supported or clamped. Differential quadrature approximation in the X-axis is employed to convert the partial differential governing equations and the associated boundary conditions into a set of ordinary differential equations. By choosing the appropriate functions as the displacement and stress functions on each nodal line and then applying the Galerkin procedure, a system of non-linear algebraic equations is obtained, from which the non-linear bending response of the plate is determined through a Picard iteration scheme. Numerical results for zirconia/aluminium rectangular plates are given in dimensionless graphical form. The effects of the applied actuator voltage, the volume fraction exponent, the temperature gradient, as well as the characteristics of the boundary conditions are also studied in detail. Copyright (C) 2004 John Wiley Sons, Ltd.

Interrogation of fibre optic sensors

The aim of the research work described in this thesis was to investigate the interrogation of fibre optic sensors using "off the shelf optical components and equipment developed mainly for the telecommunications industry. This provides a cost effective way of bringing fibre optic sensor systems to within the price range of their electro-mechanical counterparts. The research work focuses on the use of an arrayed waveguide grating, an acousto-optic tuneable filter and low-coherence interferometry to measure dynamic strain and displacement using fibre Bragg grating and interferometric sensors. Based on the intrinsic properties of arrayed waveguide gratings and acousto-optic tuneable filters used in conjunction with interferometry, fibre Bragg gratings and interferometric sensors a number of novel fibre optic sensor interrogation systems have been realised. Special single mode fibre, namely, high-birefringence fibre has been employed to implement a dual-beam interrogating interferometer. The first interrogation scheme is based on an optical channel monitor, which is an arrayed waveguide grating with integral photo-detectors providing a number of amplified electrical outputs. It is used to interrogate fibre Bragg grating and interferometric sensors. Using the properties of polarisation maintainability in high-birefringent fibre an interrogating interferometer was realised by winding a length of the fibre around a piezoelectric modulator generating a low-frequency carrier signal. The system was used to interrogate both fibre Bragg grating and interferometric sensors. Finally, the use of an acousto-optic tuneable filter is employed to interrogate fibre Bragg gratings. The device is used to generate a very high frequency carrier signal at the output of an optical interferometer.

Nanostructured piezoelectric materials for the design and development of self-sensing composite materials and energy harvesting devices

The work activities reported in this PhD thesis regard the functionalization of composite materials and the realization of energy harvesting devices by using nanostructured piezoelectric materials, which can be integrated in the composite without affecting its mechanical properties. The self-sensing composite materials were fabricated by interleaving between the plies of the laminate the piezoelectric elements. The problem of negatively impacting on the mechanical properties of the hosting structure was addressed by shaping the piezoelectric materials in appropriate ways. In the case of polymeric piezoelectric materials, the electrospinning technique allowed to produce highly-porous nanofibrous membranes which can be immerged in the hosting matrix without inducing delamination risk. The flexibility of the polymers was exploited also for the production of flexible tactile sensors. The sensing performances of the specimens were evaluated also in terms of lifetime with fatigue tests. In the case of ceramic piezo-materials, the production and the interleaving of nanometric piezoelectric powder limitedly affected the impact resistance of the laminate, which showed enhanced sensing properties. In addition to this, a model was proposed to predict the piezoelectric response of the self-sensing composite materials as function of the amount of the piezo-phase within the laminate and to adapt its sensing functionalities also for quasi-static loads. Indeed, one final application of the work was to integrate the piezoelectric nanofibers in the sole of a prosthetic foot in order to detect the walking cycle, which has a period in the order of 1 second. In the end, the energy harvesting capabilities of the piezoelectric materials were investigated, with the aim to design wearable devices able to collect energy from the environment and from the body movements. The research activities focused both on the power transfer capability to an external load and the charging of an energy storage unit, like, e.g., a supercapacitor.

Template-based fluoroethylenepropylene piezoelectrets with tubular channels for transducer applications

We describe the concept, the fabrication, and the most relevant properties of a piezoelectric-polymer system: Two fluoroethylenepropylene (FEP) films with good electret properties are laminated around a specifically designed and prepared polytetrafluoroethylene (PTFE) template at 300 degrees C. After removing the PTFE template, a two-layer FEP film with open tubular channels is obtained. For electric charging, the two-layer FEP system is subjected to a high electric field. The resulting dielectric barrier discharges inside the tubular channels yield a ferroelectret with high piezoelectricity. d(33) coefficients of up to 160 pC/N have already been achieved on the ferroelectret films. After charging at suitable elevated temperatures, the piezoelectricity is stable at temperatures of at least 130 degrees C. Advantages of the transducer films include ease of fabrication at laboratory or industrial scales, a wide range of possible geometrical and processing parameters, straightforward control of the uniformity of the polymer system, flexibility, and versatility of the soft ferroelectrets, and a large potential for device applications e.g., in the areas of biomedicine, communications, production engineering, sensor systems, environmental monitoring, etc.

Designing real nanotube-based gas sensors

Using a combination of density functional theory and recursive Green's functions techniques, we present a full description of a large scale sensor, accounting for disorder and different coverages. Here, we use this method to demonstrate the functionality of nitrogen-rich carbon nanotubes as ammonia sensors as an example. We show how the molecules one wishes to detect bind to the most relevant defects on the nanotube, describe how these interactions lead to changes in the electronic transport properties of each isolated defect, and demonstrate that there are significative resistance changes even in the presence of disorder, elucidating how a realistic nanosensor works.

Detection of catechol using mixed Langmuir-Blodgett films of a phospholipid and phthalocyanines as voltammetric sensors

The combination of metallic phthalocyanines (MPcs) and biomolecules has been explored in the literature either as mimetic systems to investigate molecular interactions or as supporting layers to immobilize biomolecules. Here, Langmuir-Blodgett (LB) films containing the phospholipid dimyristoyl phosphatidic acid (DMPA) mixed either with iron phthalocyanine (FePc) or with lutetium bisphthalocyanine (LuPc(2)) were applied as ITO modified-electrodes in the detection of catechol using cyclic voltammetry. The mixed Langmuir films of FePc + DMPA and LuPc(2) + DMPA displayed surface-pressure isotherms with no evidence of molecular-level interactions. The Fourier Transform Infrared (FTIR) spectra of the multilayer LB films confirmed the lack of interaction between the components. The DMPA and the FePc molecules were found to be oriented perpendicularly to the substrate, while LuPc(2) molecules were randomly organized. The phospholipid matrix induced a remarkable electrocatalytic effect on the phthalocyanines; as a result the mixed LB films deposited on ITO could be used to detect catechol with detection limits of 4.30 x 10(-7) and 3.34 x 10(-7) M for FePc + DMPA and LuPc(2) + DMPA, respectively. Results from kinetics experiments revealed that ion diffusion dominated the response of the modified electrodes. The sensitivity was comparable to that of other non-enzymatic sensors, which is sufficient to detect catechol in the food industry. The higher stability of the electrochemical response of the LB films and the ability to control the molecular architecture are promising for further studies with incorporation of biomolecules.

Thermodynamic modeling of pyroelectric and piezoelectric properties of cellular polymers

A thermodynamic approach is presented to model devices manufactured with cellular polymers. They are heterogeneous nonpolar space-charge electrets that exhibit much higher piezoelectricity than the well-known ferroelectric polymers. Their pyroelectric and piezoelectric properties are characterized by adequate coefficients which quantify the performance of devices manufactured with those materials. The method presented in this contribution to calculate those coefficients is exact and consistent avoiding ad hoc simplifications introduced in other approaches. The results obtained by this method allow drawing conclusions regarding device optimization.

Probing magnetic and gold nanoparticles by using MAClevers (R) as ultrasensitive sensors

Magnetic AFM probes known as MAClevers (R) were employed for sensing picogram amounts of magnetic nanoparticles, based on the cantilever frequency shifts resulting from the magnetically induced adsorption of mass. By using organothiol functionalized magnetic nanoparticles, this analytical strategy was successfully extended to the detection of gold nanoparticles, as confirmed by confocal Raman microscopy.

Effective Electromechanical Coupling Coefficients of Piezoelectric Adaptive Structures: Critical Evaluation and Optimization

This work presents a critical analysis of methodologies to evaluate the effective (or generalized) electromechanical coupling coefficient (EMCC) for structures with piezoelectric elements. First, a review of several existing methodologies to evaluate material and effective EMCC is presented. To illustrate the methodologies, a comparison is made between numerical, analytical and experimental results for two simple structures: a cantilever beam with bonded extension piezoelectric patches and a simply-supported sandwich beam with an embedded shear piezoceramic. An analysis of the electric charge cancelation effect on the effective EMCC observed in long piezoelectric patches is performed. It confirms the importance of reinforcing the electrodes equipotentiality condition in the finite element model. Its results indicate also that smaller (segmented) and independent piezoelectric patches could be more interesting for energy conversion efficiency. Then, parametric analyses and optimization are performed for a cantilever sandwich beam with several embedded shear piezoceramic patches. Results indicate that to fully benefit from the higher material coupling of shear piezoceramic patches, attention must be paid to the configuration design so that the shear strains in the patches are maximized. In particular, effective square EMCC values higher than 1% were obtained embedding nine well-spaced short piezoceramic patches in an aluminum/foam/aluminum sandwich beam.

Finite element homogenization technique for the characterization of d(15) shear piezoelectric macro-fibre composites

A finite element homogenization method for a shear actuated d(15) macro-fibre composite (MFC) made of seven layers (Kapton, acrylic, electrode, piezoceramic fibre and epoxy composite, electrode, acrylic, Kapton) is proposed and used for the characterization of its effective material properties. The methodology is first validated for the MFC active layer only, made of piezoceramic fibre and epoxy, through comparison with previously published analytical results. Then, the methodology is applied to the seven-layer MFC. It is shown that the packaging reduces significantly the shear stiffness of the piezoceramic material and, thus, leads to significantly smaller effective electromechanical coupling coefficient k(15) and piezoelectric stress constant e(15) when compared to the piezoceramic fibre properties. However, it is found that the piezoelectric charge constant d(15) is less affected by the softer layers required by the MFC packaging.