Nanoelectromechanical systems

Nanoelectromechanical systems (NEMS) are drawing interest from both technical and scientific communities. These are electromechanical systems, much like microelectromechanical systems, mostly operated in their resonant modes with dimensions in the deep submicron. In this size regime, they come with extremely high fundamental resonance frequencies, diminished active masses,and tolerable force constants; the quality (Q) factors of resonance are in the range Q~10^3–10^5—significantly higher than those of electrical resonant circuits. These attributes collectively make NEMS suitable for a multitude of technological applications such as ultrafast sensors, actuators, and signal processing components. Experimentally, NEMS are expected to open up investigations of phonon mediated mechanical processes and of the quantum behavior of mesoscopic mechanical systems. However, there still exist fundamental and technological challenges to NEMS optimization. In this review we shall provide a balanced introduction to NEMS by discussing the prospects and challenges in this rapidly developing field and outline an exciting emerging application, nanoelectromechanical mass detection

Ultra-High Frequency Nanoelectromechanical Systems with Low-Noise Technologies for Single-Molecule Mass Sensing

Advancing today's very rudimentary nanodevices toward functional nanosystems with considerable complexity and advanced performance imposes enormous challenges. This thesis presents the research on ultra-high frequency (UHF) nanoelectromechanical systems (NEMS) in combination with low-noise technologies that enable single-molecule mass sensing and offer promises for NEMS-based mass spectrometry (MS) with single-Dalton sensitivity. The generic protocol for NEMS resonant mass sensing is based on real-time locking and tracking of the resonance frequency as it is shifted by the mass-loading effect. This has been implemented in two modes: (i) creating an active self-sustaining oscillator based on the NEMS resonator, and (ii) a higher-precision external oscillator phase-locking to and tracking the NEMS resonance. The first UHF low-noise self-sustaining NEMS oscillator has been demonstrated by using a 428MHz vibrating NEMS resonator as the frequency reference. This stable UHF NEMS oscillator exhibits ~0.3ppm frequency stability and ~50zg (1zg = 10-21 g) mass resolution with its excellent wideband-operation (~0.2MHz) capability. Given its promising phase noise performance, the active NEMS oscillator technology also offers important potentials for realizing NEMS-based radio-frequency (RF) local oscillators, voltage-controlled oscillators (VCOs), and synchronized oscillators and arrays that could lead to nanomechanical signal processing and communication. The demonstrated NEMS oscillator operates at much higher frequency than conventional crystal oscillators and their overtones do, which opens new possibilities for the ultimate miniaturization of advanced crystal oscillators. Low-noise phase-locked loop (PLL) techniques have been developed and engineered to integrate with the resonance detection circuitry for the passive UHF NEMS resonators. Implementations of the NEMS-PLL mode with generations of low-loss UHF NEMS resonators demonstrate improving performance, namely, reduced noise and enhanced dynamic range. Very compelling frequency stability of ~0.02ppm and unprecedented mass sensitivity approaching 1zg has been achieved with a typical 500MHz device in the narrow-band NEMS-PLL operation. Retaining high quality factors (Q's) while scaling up frequency has become crucial for UHF NEMS resonators. Extensive measurements, together with theoretical modeling, have been performed to investigate various energy loss mechanisms and their effects on UHF devices. This leads to important insights and guidelines for device Q-engineering. The first VHF/UHF silicon nanowire (NW) resonators have been demonstrated based on single-crystal Si NWs made by bottom-up chemical synthesis nanofabrication. Pristine Si NWs have well-faceted surfaces and exhibit high Q's (Q ≈ 13100 at 80MHz and Q ≈ 5750 at 215MHz). Given their ultra-small active mass and very high mass responsivity, these Si NWs also offer excellent mass sensitivity in the ~10?50zg range. These UHF NEMS and electronic control technologies have demonstrated promising mass sensitivity for kilo-Dalton-range single-biomolecule mass sensing. The achieved performance roadmap, and that extended by next generations of devices, clearly indicates realistic and viable paths toward the single-Dalton mass sensitivity. With further elaborate engineering, prototype NEMS-MS is optimistically within reach.</p

Ühedimensionaalsete nanostruktuuride tribomehaanilised omadused: lõplike elementide meetodi simulatsioonidega toetatud eksperimentaalmõõtmised

Väitekirja elektrooniline versioon ei sisalda publikatsiooneVäitekirja raames uuriti mitmeid olulisi küsimusi, mis käsitlevad 1D nanostruktuuride mehaanilisi ja triboloogilisi omadusi ja käitumist. Põhitegevused ja uudsed aspektid on esitatud allpool. 1DNS elemente manipuleeriti tasasel pinnal ja analüüsiti vastavaid triboloogilisi protsesse. Alljärgnevalt tuvastati: • Tasasel pinnal asetsev elastselt painutatud nanotraat on väga oluline nanotriboloogilistes mõõtmistes, kuna võimaldab nanotraadi profiilist lähtuvalt leida alusega seotud triboloogilised väärtused ilma välist jõusensorit kasutamata. Meetodi täpsuse parandamiseks töötati välja uudne analüütiline meetod, mis võtab arvesse staatilise hõõrde jaotuse tasasel pinnal asetseva elastselt painutatud nanotraadil. Erinevalt varasematest meetoditest pakub uus mudel realistlikuma jõuspektri ja arvesteb ääretingimusi. Meetodit rakendati edukalt staatilise hõõrdumise arvutamiseks ZnO nanotraatide korral, mis olid ränialusel AFM-i teravikuga manipuleerimisega suvalisse kujusse painutatud. • Uus FEM mudel töötati välja sellise konfiguratsiooni jaoks, kus osa nanotraadist toetub lamedale substraadile, samal ajal kui teine osa on vabalt üle serva. Üleulatuva vaba otsa painutatakse alusele fikseeritud osa nihkumiseni. Registreerides paindprofiili vahetult enne fikseeritud osa nihkumist, saame sisendi fikseeritud osa mõjutatava jõu arvutamiseks. Vanemate mudelite puhul võeti eelduseks staatilise hõõrdejõu ühtlast jaotust fikseeritud osale. Uue mudeli puhul näidati staatilise hõõrdumise ületamist väga lokaliseeritud protsessina, mis sarnaneb pragude tekkimisega. Näidati, et olemasolevad mudelid on staatilisest hõõrdumise rolli tunduvalt alahinnatud, samas kui uus mudel pakub reaalsusega paremat kooskõla. • Töötati välja dünaamiline FEM-mudel lamedal aluspinnal asetsevast mõlemast otsast sulanud Ag nanotraadi kirjeldamiseks. Näidati, et nanotraadis tekitatud mehaanilised pinged on tingitud asjaolust, et sulanud otsad moodustavad ümarad elemendid, mille tulemusena on võimalik ületada nanotraadi ja ränialuse vahelist adhesiooni. Selle tulemusena saavutatakse konfiguratsioon, kus ainult saadud nanoosakeste otsaelmemendid puutuvad kokku pinnaga, samas kui keskosa on pinna kohal. Selline “hantlisarnane” struktuur ja konfiguratsioon on tribologiliste mõõtmiste jaoks äärmiselt atraktiivne, kuna seda saab hõlpsasti manipuleerida väikese kontaktiala tõttu ja samal ajal säilivad kõik 1D geomeetria eelised. Lisaks uuriti alljärgnevid 1DNS mehaanilisi omadusi: • Karakteriseeriti paksude seintega torukujuliste 1DNS elastseid omadusi kasutades nii eksperimentaalseid kui ka teoreetili meetodeid. o SiO2 nanotorude elastset moodulit mõõdeti kolme erineva meetodi abil, kasutades konsooltala painutamist, nanoindetatsiooni ja kolme punkti paindekatseid. Tuvastati, et kolme punkti paindekatse on kõige täpsem meetod paksuseinaliste torukujuliste 1DNS elastusmooduli mõõtmiseksA number of important issues concerning mechanical and tribological properties and behavior of 1D nanostructures were studied within the framework of the thesis. Main activity and the novelty aspects are summarized below. First, tribological aspects of 1DNS manipulated on a flat substrate were considered. In particular: • Nanowire elastically bent of a flat substrate is highly attractive for nanotribological studies as profile of nanowire can be used for extracting frictional data without using external force sensors. In order to improve accuracy of the method, a novel analytical method was developed for the calculation of distributed static friction in elastically bent nanowire resting on a flat substrate. Unlike previously available methods, new model provides more realistic force spectrum and comply with boundary conditions. The method was successfully applied for calculation of distributed static friction in ZnO nanowires bent into arbitrary shapes in AFM manipulations on a Si substrate. • A novel FEM model was developed for configuration in which part of the nanowire is resting on a flat substrate while other part is suspended over the trench. Measurements consist in bending the free end until fixed part is displaced. The bending profile prior the displacement of fixed part is used for calculation of force acting on a fixed part. In older models static friction was considered to be uniformly distributed in adhered part. The new model considered overcoming of static friction as a highly localized process similar to crack formation. It was shown, that existing models severely underestimated static friction, while novel model provides more realistic results. • Dynamic FEM model of Ag nanowire that is being melted from both ends while resting on a flat substrate was created. It was shown that mechanical stresses, generated in nanowire due to the fact that molted ends form rounded bulbs, are able to overcome the adhesion between nanowire and silicon substrate. As a result, a configuration is achieved where only the end-bulbs of the obtained nanodumbell are in contact with the surface while intact midpart is suspended above the substrate. Such structure and configuration is highly attractive for tribological measurements as it can be easily manipulated due to the small contact area and at the same time it preserves all benefits of 1D geometry. Further, mechanical properties of 1DNS were considered: • Elastic properties of tubular 1DNS with thick walls were treated both experimentally and theoretically. o Elastic modulus of SiO2 nanotubes was measured by three different methods including cantilever beam bending, nanoindentation and three-point bending tests. Three-point bending tests were found to be the most appropriate method for measuring the Young’s modulus of thick-walled tubular 1DNS. o FEM model was created to investigate the behavior of tubular 1DNS in nanoindentation test. It was shown there are both compression and indentation present. Thus, neither of existing models where walls of nanotube are considered either as a thin membrane or rigid wall cannot be used for given system as they underestimate the Young modulus. • FEM model of composite core-shell nanowire consisting of elastic core and viscous shell was created to simulate the behavior of Ag/SiO2 core-shell nanowire in bending test under electron beam irradiation. By fitting the experimental result with FEM model it was found that even at moderate current and voltage e-beam is capable of inducing glass transition in amorphous oxide shell. Finally, two variations of three-point bending test of Au nanowires were compared: freely sliding ends and rigidly fixed ends. The effect of different boundary conditions on experimental results was determined and the adhesion forces acting between Au and substrate were estimated using the FEM modeling. In total, it was demonstrated that FEM is a powerful method for studying mechanical and tribological properties of nanoscale systems when used in combination with experimental result

Microwave Dielectrometry Adapted to Environments

Tesis por compendio[ES] La permitividad es una propiedad física de los materiales que describe su comportamiento en presencia de un campo electromagnético. Los sensores de microondas pueden desempeñar un papel esencial en las tareas de detección, supervisión o control de procesos, ya que algunos parámetros fisicoquímicos de los materiales producen cambios medibles en las propiedades dieléctricas. Además, la tecnología de calentamiento por microondas está adquiriendo una relevancia creciente para la transición ecológica y la descarbonización de los procesos industriales, y la permitividad es el parámetro esencial para el desarrollo exitoso de estos nuevos procesos. La permitividad depende de muchos factores, por lo que los métodos de medición de la permitividad deben adaptarse a las necesidades del material y del entorno de medición. El número de aplicaciones que requieren la monitorización o medida de las propiedades dieléctricas, las altas dependencias de esta magnitud bajo diferentes condiciones, y la necesidad de poner esta tecnología al alcance de un usuario más amplio y menos especializado, justifican el desarrollo de este trabajo. Esta tesis pretende desarrollar nuevos dispositivos para la monitorización y caracterización de dieléctricos adaptados a diferentes entornos, cubriendo un amplio rango de formatos, formas y propiedades de los materiales. Las dos primeras publicaciones incluidas en la tesis describen dos enfoques diferentes para abordar las mediciones de permitividad. El primer artículo describe un instrumento versátil, autónomo y fácil de usar para medir la permitividad de materiales dentro de tubos. El diseño de la cavidad logró una excelente sensibilidad, y el estudio de la red de acoplamiento permitió la caracterización de materiales de pérdidas bajas, moderadas y altas con una misma configuración. Este dispositivo incluye un reflectómetro vectorial portátil propio, lo que lo hace portátil y asequible. Las características del instrumento desarrollado permiten un uso sencillo por parte de personal no especializado y proporcionan versatilidad en muchas situaciones. La segunda publicación presenta el diseño específico de una sonda coaxial de extremo abierto con una mayor sensibilidad para determinar la permitividad de productos alimenticios de altas pérdidas en función de la temperatura a frecuencias de RF. Este artículo destaca la importancia de seleccionar la técnica de medición más adecuada, adaptada al entorno y a las particularidades del material, para la determinación apropiada de la permitividad. Los dos artículos siguientes describen el desarrollo y la utilización de un microscopio de microondas de campo cercano con resolución micrométrica para determinar mapas de permitividad de materiales planos heterogéneos a frecuencias de microondas. En ambos trabajos se describen los diferentes elementos que componen el instrumento del microscopio y las técnicas de análisis para determinar los valores de permitividad a partir de las medidas de los parámetros de la resonancia. En el primer trabajo se empleó por primera vez la tecnología de microondas en aplicaciones contra la falsificación, obteniendo la marca dieléctrica de la marca de agua de un billete. Además, este estudio demostró la capacidad de la energía de microondas para detectar marcas ocultas detrás de capas dieléctricas o metálicas, lo que abre nuevas posibilidades para el desarrollo de elementos de seguridad ópticamente opacos e imposibles de rastrear por medios ópticos. El segundo estudio demuestra la versatilidad de este sistema para determinar las propiedades dieléctricas de materiales planos heterogéneos midiendo la respuesta dieléctrica de especímenes de roca. Los métodos desarrollados en esta tesis aumentan la cartera de sistemas de caracterización dieléctrica y pueden ayudar a una amplia gama de sectores científicos e industriales en las tareas de monitorización y caracterización dieléctrica, haciendo estos trabajos más cómodos y accesibles.[CA] La permitivitat és una propietat física dels materials que descriu el seu comportament en presència d'un camp electromagnètic. Els sensors de microones poden exercir un paper essencial en les tasques de detecció, supervisió o control de processos, ja que alguns paràmetres fisicoquímics dels materials produeixen canvis mesurables en les propietats dielèctriques. A més, la tecnologia de calfament per microones està adquirint una rellevància creixent per a la transició ecològica i la descarbonització dels processos industrials, i la permitivitat és el paràmetre essencial per al desenvolupament reeixit d'aquests nous processos. La permitivitat depén de molts factors i, per tant, els mètodes de mesurament de la permitivitat han d'adaptar-se a les necessitats del material i de l'entorn de mesurament. El nombre d'aplicacions que requereixen el monitoratge o mesura de les propietats dielèctriques, les altes dependències d'aquesta magnitud sota diferents condicions, i la necessitat de posar aquesta tecnologia a l'abast d'un usuari més ampli i menys especialitzat, justifiquen el desenvolupament d'aquest treball. Aquesta tesi pretén desenvolupar nous dispositius per al monitoratge i caracterització de dielèctrics adaptats a diferents entorns, cobrint un ampli rang de formats, formes i propietats dels materials. Les dues primeres publicacions incloses en la tesi descriuen dos enfocaments diferents per a abordar els mesuraments de permitivitat. El primer article descriu un instrument versàtil, autònom i fàcil d'usar per a mesurar la permitivitat de materials dins de tubs. El disseny de la cavitat va aconseguir una excel·lent sensibilitat, i l'estudi de la xarxa d'acoblament va permetre la caracterització de materials de pèrdues baixes, moderades i altes amb una mateixa configuració. Aquest dispositiu inclou un reflectòmetre vectorial portàtil propi, la qual cosa el fa portàtil i assequible. Les característiques de l'instrument desenvolupat permeten un ús senzill per part de personal no especialitzat i proporcionen versatilitat en moltes situacions. La segona publicació presenta el disseny específic de una sonda coaxial d'extrem obert amb una major sensibilitat per a determinar la permitivitat de productes alimentaris d'altes pèrdues en funció de la temperatura a freqüències de RF. Aquest article destaca la importància de seleccionar la tècnica de mesurament més adequat, adaptada a l'entorn i a les particularitats del material, per a la determinació apropiada de la permitivitat. Els dos articles següents descriuen el desenvolupament i la utilització d'un microscopi de microones de camp pròxim amb resolució micromètrica per a determinar mapes de permitivitat de materials plans heterogenis a freqüències de microones. En tots dos treballs es descriuen els diferents elements que componen l'instrument del microscopi i les tècniques d'anàlisis per a determinar els valors de permitivitat a partir de les mesures dels paràmetres de la ressonància. En el primer treball es va emprar per primera vegada la tecnologia de microones en aplicacions contra la falsificació, obtenint la marca dielèctrica de la marca d'aigua d'un bitllet. A més, aquest estudi va demostrar la capacitat de l'energia de microones per a detectar marques ocultes darrere de capes dielèctriques o metàl·liques, la qual cosa obri noves possibilitats per al desenvolupament d'elements de seguretat òpticament opacs i impossibles de rastrejar per mitjans òptics. El segon estudi demostra la versatilitat d'aquest sistema per a determinar les propietats dielèctriques de materials plans heterogenis mesurant la resposta dielèctrica d'espècimens de roca. Els mètodes desenvolupats en aquesta tesi augmenten la cartera de sistemes de caracterització dielèctrica i poden ajudar a una àmplia gamma de sectors científics i industrials en les tasques de monitoratge i caracterització dielèctrica, fent aquests treballs més còmodes i accessibles.[EN] Permittivity is a physical property of materials describing their behavior in the presence of an electromagnetic field. Microwave sensors can play an essential role in detecting, monitoring, or process control tasks as some physicochemical parameters of materials produce measurable changes in dielectric properties. Besides, microwave heating technology is gaining increasing relevance for the ecological transition and decarbonization of industrial processes, and permittivity is the essential parameter for the successful development of these new processes. Permittivity depends on many factors and thus, permittivity measurement methods must be adapted to the needs of the material and the measurement environment. The number of applications that require the monitoring or measurement of dielectric properties, the high dependencies of this magnitude under different conditions, and the need to make this technology available to a broader and less specialized user justify the development of this work. This thesis aims to develop new devices for the monitoring and characterization of dielectrics adapted to different environments, covering a wide range of materials' formats, shapes, and properties. The first two publications included in the thesis describe two different approaches to address permittivity measurements. The first paper describes a versatile, stand-alone, and easy-to-use instrument for measuring the permittivity materials inside tubes. The design of the cavity achieved an excellent sensitivity, and the study of the coupling network allowed the characterization of low, moderate, and high-loss materials with the same setup. This device included an in-house portable vector reflectometer, making it portable and cost-affordable. The features of the developed instrument allow straightforward use by non-specialized personnel and provide versatility in many situations. The second publication presents a specific open-ended coaxial design with increased sensitivity to determine the permittivity of lossy food products as a function of temperature at RF frequencies. This paper highlight the relevance of selecting the most suitable measurement technique, adapted to the environment and particularities of the material, for the appropriate determination of permittivity. The following two papers describe the development and use of a near-field scanning microwave microscope with micrometric resolution to determine permittivity maps of heterogeneous planar materials at microwave frequencies. The different elements comprising the microscope instrument and the analysis techniques to determine permittivity values from the resonance measurements were described throughout both works. In the first paper, microwave technology was employed for the first time in anti-counterfeiting applications by obtaining the dielectric mark of a banknote watermark. Besides, this study showed the ability of microwave energy to detect hidden marks behind dielectric or metallic layers, opening new possibilities for developing optically opaque security features untraceable by optical means. The second study demonstrates the versatility of this system in determining the dielectric properties of heterogeneous planar materials by measuring the dielectric response of rock specimens. The methods developed in this thesis dissertation increase the portfolio of dielectric characterization systems and can help a wide range of scientific and industrial sectors in dielectric monitoring and characterization tasks, making these works more convenient and accessible.Financial support through the grant reference BES-2016-077296 of the call Convocatoria de las ayudas para contratos predoctorales para la formación de doctores de 2016 by Ministerio de Economía y Competitividad (MINECO) and by European Social Funds (ESF) of European Union is also gratefully acknowledgedGutiérrez Cano, JD. (2022). Microwave Dielectrometry Adapted to Environments [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/186351TESISCompendi