Nouveau concept de spectrométre de masse à base de réseaux de nanostructures résonantes

The aim of the project is to bring a proof of concept of a simplified mass spectrometer architecture using an ultra dense network of NEMS in association with elements of CMOS circuit as sensors in order to amplify the signal in situ and adress them individually. Since several years, Roukes' team at Caltech has demonstrated a mass spectrometry with a NEMS. In parallel, the CEA/LETI-MINATEC has developped a fabrication approach called VLSI of NEMS and an electromecanical simulation method of these elements The first objective of this thesis is to study the noise phenomenon currently limiting our mass resolution in order to reach 10 Da instead of current 1000 Da on ranges going from 10 Da to 1MDa. In a second step, the concept of NEMS-based mass spectrometry is validated by comparison a nanometric cluster spectra with those from a conventional time-of-flight mass spectrometer. Then, a frequency addressing technique is applied on an NEMS array to allow for quasi simultaneous tracking of 20 different resonators. Finally, the NEMS array is inserted in the nanocluster bench to measure 20 spectra in parallel and validate a first proof of concept.L'enjeu du travail est d'apporter une preuve de concept d'une architecture simplifiée de spectromètre en utilisant comme détecteur un réseau ultra-dense de NEMS associés à des éléments de circuit CMOS afin d'amplifier le signal in situ et de les adresser individuellement. Depuis plusieurs années, l'équipe du professeur Roukes à CALTECH a présenté une démonstration de spectrométrie de masse avec un NEMS. En parallèle, le CEA/LETI-MINATEC a développé une approche de fabrication dite VLSI de NEMS et de simulation électromécanique de ces éléments. Le premier but de la thèse est l'étude des phénomènes de bruit limitant la résolution en masse afin d'atteindre 10 Da au lieu des 1000 Da actuels sur des rangs de masses large allant de 10Da à 1MDa. Dans un second temps, La concept de spectrométrie de masse à base de NEMS est validé en comparant des spectres obtenus sur des nano-agrégats de quelques nanomètres de diamètres avec ceux fournis par un spectromètre de masse temps-de-vol conventionnel. Puis, un système d'adressage fréquentiel de réseau de NEMS est mis en place pour permettre la mesure quasi simultanée de 20 résonateurs. Enfin, le réseau de NEMS est inséré dans le banc de nano-aggrégats pour mesurer 20 spectres de masses en parallèle et valider une première preuve de concept

Micro-poutres résonantes à base de films minces de nitrure d’aluminium piézoélectriques, application aux capteurs de gaz gravimétriques

Resonant MEMS and NEMS are excellent candidate for the realization of low cost and high resolution gas sensing systems that have several applications in security, defense, and environment and health care domains. However, the question of the transduction technique used to couple micro or nano scale signals to the macro scale is still a key issue. Piezoelectric transduction can be advantageously exploited but has been rarely studied at the nano-scale. The objective of this PhD is thus to progress toward the realization of high-resolution gas sensor using piezoelectric micro/nano cantilevers resonators and cover the whole prototyping chain from device fabrication to proof of principle experiment. Our first contribution in this research relates the analytical modeling of the sensing performance and the system and design optimization. In particular we demonstrate that decreasing the piezoelectric active film thickness below 100 nm is particularly beneficial. The second contribution relates the fabrication, characterization and demonstration of the high sensing performances of 80 μm long cantilevers embedding a 50 nm thick piezoelectric AlN film for transduction. These devices exhibit state of the art performances in terms of resonance frequency deviation down to the 〖10〗^(-8) range. They allow thus the detection of Di-Methyl-Methyl-Phosphonate vapors, a sarin gas simulant, with concentration as low as 10 ppb. Although the level of integration of our sensing system is not sufficient for real life application, these results prove the high potential of these piezoelectric cantilever resonators for future industrial development.Les MEMS et NEMS résonants sont d'excellents candidats pour la réalisation de systèmes de détection de gaz haute résolution et faible couts ayant des applications dans les domaines de la sécurité, la défense, l'environnement et la santé. Cependant, la question du choix des techniques de transduction est toujours largement débattue. La transduction piézoélectrique pourrait être avantageusement exploitée mais elle est encore peu connue à l'échelle nanométrique. L'objectif de cette thèse est donc de progresser vers la réalisation de capteur de gaz à haute résolution à l'aide résonateurs à base de micro / nano poutres piézoélectriques en couvrant la chaîne de prototypage complète depuis les techniques de dépôt des matériaux jusqu'à l'expérience de preuve de principe de mesure de gaz. Pour cela, notre première contribution concerne la modélisation analytique des performances et l'optimisation, design et système, d'un capteur de gaz à base de poutres résonantes piézoélectriques. En particulier, nous démontrons que la diminution de l'épaisseur du film piézoélectrique actif sous la barre des 100 nm permet d'atteindre les meilleures performances. La deuxième contribution concerne la fabrication, la caractérisation et la démonstration des performances capteur de poutres résonantes de 80 μm de long exploitant un film piézoélectrique en AlN de 50 nm d'épais. Ainsi nous avons démontré expérimentalement la stabilité fréquentielle exceptionnelle de ces dispositifs atteignant des déviations standard de l'ordre de 〖10〗^(-8), au niveau de l’état de l'art. Ainsi, ils permettent la détection de vapeurs Di -Methyl -méthyl- phosphonates, un simulateur de gaz sarin, avec des concentrations aussi faibles que 10 ppb. Bien que le niveau d'intégration de notre système de détection ne soit pas suffisant, ces résultats prouvent le fort potentiel de ces résonateurs cantilever piézoélectriques pour un développement industriel futur

Towards Single Molecule Imaging Using Nanoelectromechanical Systems

We incorporate nanoelectromechanical systems (NEMS) into a state-of-the-art commercial mass spectrometer (Q Exactive Plus with Orbitrap detection). This unique hybrid instrument is capable of ionizing molecules up to 4.5 MDa in their intact native state, isolating molecules of interest according to their mass-to-charge ratio, performing high resolution mass spectrometry (MS), and delivering those molecules to the NEMS. We use NEMS optimized for detecting the inertial mass of adsorbed species directly, which contrasts with indirect measurements of the mass-to-charge ratio performed with typical instruments. This unique form of mass spectrometry, NEMS-MS, with its single-molecule sensitivity, has promising applications to the fields of proteomics and native mass spectrometry, including deep proteomic profiling, single-cell proteomics, mass spectrometry-based imaging, or identifying viruses in their in vivo state. We analyze intact E. coli GroEL chaperonin, a noncovalent 801 kDa complex consisting of 14 identical subunits. GroEL was sent to NEMS operated with the first two vibrational modes monitored in real time. Molecules physisorbing to the NEMS cause an abrupt shift in its resonance frequencies. The change in resonance frequencies is used to calculate the mass of each molecule. A mass spectrum is compiled with a main peak of 846 kDa, close to the expected value, and a secondary peak resolved near twice the mass of GroEL. Measurements are then performed operating the first three modes simultaneously. Using a technique called inertial imaging, frequency shifts are used to calculate the first three mass moments: mass, position, and variance (size). This is used to distinguish between adsorbates arriving in a single, point-like distribution or a more extended distribution, thus demonstrating a rudimentary form of molecular imaging. Two new theories are presented for analyzing frequency-shift data. The first approach offers a more streamlined approach for calculating the mass moments. This approach is used to improve the mass spectrum of the GroEL calculated using three-mode data, producing a main peak almost fully resolved at 805 kDa. An entirely different approach is presented that allows for obtaining the mass density distribution of an adsorbed molecule (i.e., imaging) with a higher number of modes.</p

Focused electron- and ion-beam induced processes:in situ monitoring, analysis and modeling

Focused electron- and ion-beam induced processing are well established techniques for local deposition and etching that rely on decomposition of precursor molecules by irradiation. These high-resolution nanostructuring techniques have various applications in nanoscience including attach-and-release procedures in nanomanipulation and fabrication of sensors (magnetic, optical and thermal) for scanning probe microscopy. However, a complete physical and chemical understanding of the process is hampered by the lack of suitable means to monitor and to access the numerous interrelated and time-varying process parameters (deposition and etch rate, yield, molecule flux and adsorption/desorption). This thesis is a first attempt to fill this gap. It is based on experimental and simulative approaches for the determination of process conditions and mechanical properties of deposited materials: Mass and force sensors: The use of tools merging micromechanical cantilever sensors and scanning electron microscopy was demonstrated for in situ monitoring and analysis. A cantilever-based resonant mass sensing setup was developed and used for real-time mass measurements. A noise level at the femtogram-scale was achieved by tracking the resonance frequency of a temperature stabilized piezoresistive cantilever using phase-locking. With this technique the surface coverage and residence time of (CH3)3PtCpCH3 molecules, the mass deposition rate, the yield, and the material density of corresponding deposits were measured. In situ cantilever-based static force sensing and mechanical modal vibration analysis were employed to investigate the Young's modulus and density of individual high aspect ratio deposits from the precursor Cu(hfac)2. Precursor supply simulations and experiments: A prerequisite to understand and quantify irradiative precursor chemistry is the knowledge of the local flux of molecules impinging on the substrate. Therefore, Monte Carlo simulations of flux distributions were developed and gas flows injected into a vacuum chamber were analyzed experimentally for the precursors Co2(CO)8, (hfac)CuVTMS, and [(PF3)2RhCl]2. The process parameters extracted from the mentioned approaches are valuable input for numerical focused electron- and ion-beam induced process models (Monte Carlo, continuum). We evaluated the precursor surface diffusion coefficient and the electron impact dissociation cross-section by relating deposit shapes to a continuum model

Towards Ultra-High Resolution Mode-localised MEMS Sensors

Sensors employing mode localisation in weakly coupled resonators have been increasingly viewed as an alternative to resonant frequency shift based sensing. Much theory has been proposed highlighting the advantages of these sensors including the increased sensitivity and the promise of common mode rejection to first order environmental variations. This has led to the development of proof-of-concept sensors to sense physical quantities such as displacement, charge, mass, and acceleration. However, practical aspects of developing a sensor starting from design of a closed-loop implementation to understanding different operating regions with the aim of resolution analysis and noise optimisation have yet to be explored in depth. This work delves into these practical aspects of developing ultra-high resolution mode-localised MEMS sensors. First, the mechanical sensor is integrated with a prototype closed-loop oscillator along with the interface electronics on a printed circuit board. Key aspects of sensors such as stability, noise floor, and bandwidth are analysed using this integrated sensor system. A critical observation is made on the improvement of stability of the amplitude ratio output metric over its frequency shift counterpart at large integration times therefore, highlighting the advantage of common mode rejection to environmental factors. The common mode rejection abilities of both mechanically and electrically coupled devices are next studied at different operating regions. These are then compared to the state-of-the-art differential frequency measurements. Amplitude ratio measurements in an electrically coupled device showed an order of magnitude better rejection to temperature variations over a mechanically coupled device. Furthermore, amplitude ratio measurements in the electrically coupled device were on par with the rejection offered by the differential frequency output in the same device. This result highlights the advantage of amplitude ratio measurements that are able to achieve the same common mode rejection with the help of a single oscillator instead of the two oscillators required in differential frequency output measurements. The resolution of the mode-localised sensor is then explored with the purpose of optimising operating regions to achieve the best noise figure. A detailed theoretical analysis is first undertaken to optimise the amplitude ratio noise in different noise dominant regimes. It is predicted that the resonator-based noise (such as thermo-mechanical noise) can be optimised be operating at an amplitude ratio of $\sqrt{2}$ and the electronic sourced noises can be optimised at an amplitude ratio of $\sqrt{1.5}$ in a single ended resonator drive configuration. Additionally, both sources of noise are predicted to decrease with the decrease of the coupling stiffness. This result is then validated using experimental data to verify the claim. A further noise reduction is sought by operating the coupled resonators in the nonlinear domain with interesting observations on the variations of the amplitude ratio output metric. The phase filtering offered by the bifurcation points in the nonlinear domain is utilised to further improve the noise by 4 times. Finally, a mode-localised accelerometer design is proposed that employs a novel differential amplitude ratio output metric. Noise optimisation techniques are then used to optimise this novel output metric. A noise floor of $3$ $\mu$g/\sqrt{\mbox{Hz}} with a stability of $3$ $\mu$g is achieved thus, benchmarking the mode-localised accelerometer favourably with respect to other high-end commercial MEMS accelerometers. Additionally, their potential is demonstrated with a measurement of seismic activity. This measurement is then compared to reference data sourced from an accelerometer from the British Geological Survey. Lastly, suggestions are made to further optimise the resolution in the accelerometer to push the limits of amplitude ratio sensing thereby, putting mode-localised accelerometers at par with the best resonant accelerometers till date.Innovate UK Natural Environment Research Counci

Single-Chip Scanning Probe Microscopes

Scanning probe microscopes (SPMs) are the highest resolution imaging instruments available today and are among the most important tools in nanoscience. Conventional SPMs suffer from several drawbacks owing to their large and bulky construction and to the use of piezoelectric materials. Large scanners have low resonant frequencies that limit their achievable imaging bandwidth and render them susceptible to disturbance from ambient vibrations. Array approaches have been used to alleviate the bandwidth bottleneck; however as arrays are scaled upwards, the scanning speed must decline to accommodate larger payloads. In addition, the long mechanical path from the tip to the sample contributes thermal drift. Furthermore, intrinsic properties of piezoelectric materials result in creep and hysteresis, which contribute to image distortion. The tip-sample interaction signals are often measured with optical configurations that require large free-space paths, are cumbersome to align, and add to the high cost of state-of-the-art SPM systems. These shortcomings have stifled the widespread adoption of SPMs by the nanometrology community. Tiny, inexpensive, fast, stable and independent SPMs that do not incur bandwidth penalties upon array scaling would therefore be most welcome. The present research demonstrates, for the first time, that all of the mechanical and electrical components that are required for the SPM to capture an image can be scaled and integrated onto a single CMOS chip. Principles of microsystem design are applied to produce single-chip instruments that acquire images of underlying samples on their own, without the need for off-chip scanners or sensors. Furthermore, it is shown that the instruments enjoy a multitude of performance benefits that stem from CMOS-MEMS integration and volumetric scaling of scanners by a factor of 1 million. This dissertation details the design, fabrication and imaging results of the first single-chip contact-mode AFMs, with integrated piezoresistive strain sensing cantilevers and scanning in three degrees-of-freedom (DOFs). Static AFMs and quasi-static AFMs are both reported. This work also includes the development, fabrication and imaging results of the first single-chip dynamic AFMs, with integrated flexural resonant cantilevers and 3 DOF scanning. Single-chip Amplitude Modulation AFMs (AM-AFMs) and Frequency Modulation AFMs (FM-AFMs) are both shown to be capable of imaging samples without the need for any off-chip sensors or actuators. A method to increase the quality factor (Q-factor) of flexural resonators is introduced. The method relies on an internal energy pumping mechanism that is based on the interplay between electrical, mechanical, and thermal effects. To the best of the author’s knowledge, the devices that are designed to harness these effects possess the highest electromechanical Qs reported for flexural resonators operating in air; electrically measured Q is enhanced from ~50 to ~50,000 in one exemplary device. A physical explanation for the underlying mechanism is proposed. The design, fabrication, imaging, and tip-based lithographic patterning with the first single-chip Scanning Thermal Microscopes (SThMs) are also presented. In addition to 3 DOF scanning, these devices possess integrated, thermally isolated temperature sensors to detect heat transfer in the tip-sample region. Imaging is reported with thermocouple-based devices and patterning is reported with resistive heater/sensors. An “isothermal electrothermal scanner” is designed and fabricated, and a method to operate it is detailed. The mechanism, based on electrothermal actuation, maintains a constant temperature in a central location while positioning a payload over a range of >35μm, thereby suppressing the deleterious thermal crosstalk effects that have thus far plagued thermally actuated devices with integrated sensors. In the thesis, models are developed to guide the design of single-chip SPMs and to provide an interpretation of experimental results. The modelling efforts include lumped element model development for each component of single-chip SPMs in the electrical, thermal and mechanical domains. In addition, noise models are developed for various components of the instruments, including temperature-based position sensors, piezoresistive cantilevers, and digitally controlled positioning devices

Advanced Syncom - Syncom II summary report

Spacecraft systems design, reliability, support equipment, alternate configurations, and radiation instrumentation payload for Syncom I

MEMS Accelerometers

Micro-electro-mechanical system (MEMS) devices are widely used for inertia, pressure, and ultrasound sensing applications. Research on integrated MEMS technology has undergone extensive development driven by the requirements of a compact footprint, low cost, and increased functionality. Accelerometers are among the most widely used sensors implemented in MEMS technology. MEMS accelerometers are showing a growing presence in almost all industries ranging from automotive to medical. A traditional MEMS accelerometer employs a proof mass suspended to springs, which displaces in response to an external acceleration. A single proof mass can be used for one- or multi-axis sensing. A variety of transduction mechanisms have been used to detect the displacement. They include capacitive, piezoelectric, thermal, tunneling, and optical mechanisms. Capacitive accelerometers are widely used due to their DC measurement interface, thermal stability, reliability, and low cost. However, they are sensitive to electromagnetic field interferences and have poor performance for high-end applications (e.g., precise attitude control for the satellite). Over the past three decades, steady progress has been made in the area of optical accelerometers for high-performance and high-sensitivity applications but several challenges are still to be tackled by researchers and engineers to fully realize opto-mechanical accelerometers, such as chip-scale integration, scaling, low bandwidth, etc

Microelectromechanical Systems and Devices

The advances of microelectromechanical systems (MEMS) and devices have been instrumental in the demonstration of new devices and applications, and even in the creation of new fields of research and development: bioMEMS, actuators, microfluidic devices, RF and optical MEMS. Experience indicates a need for MEMS book covering these materials as well as the most important process steps in bulk micro-machining and modeling. We are very pleased to present this book that contains 18 chapters, written by the experts in the field of MEMS. These chapters are groups into four broad sections of BioMEMS Devices, MEMS characterization and micromachining, RF and Optical MEMS, and MEMS based Actuators. The book starts with the emerging field of bioMEMS, including MEMS coil for retinal prostheses, DNA extraction by micro/bio-fluidics devices and acoustic biosensors. MEMS characterization, micromachining, macromodels, RF and Optical MEMS switches are discussed in next sections. The book concludes with the emphasis on MEMS based actuators