Sébastien Hentz

Single-protein nanomechanical mass spectrometry in real time

Nanoelectromechanical systems (NEMS) resonators can detect mass with exceptional sensitivity. Previously, mass spectra from several hundred adsorption events were assembled in NEMS-based mass spectrometry using statistical analysis. Here, we report the first realization of single-molecule NEMS-based mass spectrometry in real time. As each molecule in the sample adsorbs upon the NEMS resonator, its mass and the position-of-adsorption are determined by continuously tracking two driven vibrational modes of the device. We demonstrate the potential of multimode NEMS-based mass spectrometry by analyzing IgM antibody complexes in real-time. NEMS-MS is a unique and promising new form of mass spectrometry: it can resolve neutral species, provides resolving power that increases markedly for very large masses, and allows acquisition of spectra, molecule-by-molecule, in real-time.

Nonlinear dynamics of nanomechanical beam resonators: improving the performance of NEMS-based sensors.

In order to compensate for the loss of performance when scaling resonant sensors down to NEMS, it proves extremely useful to study the behavior of resonators up to very high displacements and hence high nonlinearities. This work describes a comprehensive nonlinear multiphysics model based on the Euler-Bernoulli equation which includes both mechanical and electrostatic nonlinearities valid up to displacements comparable to the gap in the case of an electrostatically actuated doubly clamped beam. Moreover, the model takes into account the fringing field effects, significant for thin resonators. The model has been compared to both numerical integrations and electrical measurements of devices fabricated on 200 mm SOI wafers; it shows very good agreement with both. An important contribution of this work is the provision for closed-form expressions of the critical amplitude and the pull-in domain initiation amplitude including all nonlinearities. This model allows designers to cancel out nonlinearities by tuning some design parameters and thus gives the possibility to drive the resonator beyond its critical amplitude. Consequently, the sensor performance can be enhanced to the maximum below the pull-in instability, while keeping a linear behavior.

Piezoelectric nanoelectromechanical resonators based on aluminum nitride thin films

We demonstrate piezoelectrically actuated, electrically tunable nanomechanical resonators based on multilayers containing a 100-nm-thin aluminum nitride (AlN) layer. Efficient piezoelectric actuation of very high frequency fundamental flexural modes up to ~80 MHz is demonstrated at room temperature. Thermomechanical fluctuations of AlN cantilevers measured by optical interferometry enable calibration of the transduction responsivity and displacement sensitivities of the resonators. Measurements and analyses show that the 100 nm AlN layer employed has an excellent piezoelectric coefficient, d_(31)=2.4 pm/V. Doubly clamped AlN beams exhibit significant frequency tuning behavior with applied dc voltage.

In-plane nanoelectromechanical resonators based on silicon nanowire piezoresistive detection.

We report an actuation/detection scheme with a top-down nanoelectromechanical system (NEMS) for frequency shift based sensing applications with outstanding performance. It relies on electrostatic actuation and piezoresistive nanowire gauges for in-plane motion transduction. The process fabrication is fully CMOS (complementary metal-oxide-semiconductor) compatible. The results show a very large dynamic range of more than 100 dB and an unprecedented signal to background ratio of 69 dB providing an improvement of two orders of magnitude in the detection efficiency presented in the state of the art in NEMS fields. Such a dynamic range results from both negligible 1/f noise and very low Johnson noise compared to the thermomechanical noise. This simple low power detection scheme paves the way for new class of robust mass resonant sensors.

Large-Scale Integration of Nanoelectromechanical Systems for Gas Sensing Applications

We have developed arrays of nanomechanical systems (NEMS) by large-scale integration, comprising thousands of individual nanoresonators with densities of up to 6 million NEMS per square centimeter. The individual NEMS devices are electrically coupled using a combined series-parallel configuration that is extremely robust with respect to lithographical defects and mechanical or electrostatic-discharge damage. Given the large number of connected nanoresonators, the arrays are able to handle extremely high input powers (>1 W per array, corresponding to <1 mW per nanoresonator) without excessive heating or deterioration of resonance response. We demonstrate the utility of integrated NEMS arrays as high-performance chemical vapor sensors, detecting a part-per-billion concentration of a chemical warfare simulant within only a 2 s exposure period.

Dynamic range enhancement of nonlinear nanomechanical resonant cantilevers for highly sensitive NEMS gas/mass sensor applications

This paper describes a comprehensive nonlinear multiphysics model based on the Euler–Bernoulli equation that remains valid up to large displacements in the case of electrostatically actuated nanocantilevers. This purely analytical model takes into account the fringing field effects which are significant for thin resonators. Analytical simulations show very good agreement with experimental electrical measurements of silicon nanodevices using wafer-scale nanostencil lithography (nSL), monolithically integrated with CMOS circuits. Close-form expressions of the critical amplitude are provided in order to compare the dynamic ranges of NEMS cantilevers and doubly clamped beams. This model allows designers to cancel out nonlinearities by tuning some design parameters and thus gives the possibility of driving the cantilever beyond its critical amplitude. Consequently, the sensor performance can be enhanced by being optimally driven at very large amplitude, while maintaining linear behavior.

Neutral particle mass spectrometry with nanomechanical systems

Current approaches to mass spectrometry (MS) require ionization of the analytes of interest. For high-mass species, the resulting charge state distribution can be complex and difficult to interpret correctly. Here, using a setup comprising both conventional time-of-flight MS (TOF-MS) and nano-electromechanical systems-based MS (NEMS-MS) in situ, we show directly that NEMS-MS analysis is insensitive to charge state: the spectrum consists of a single peak whatever the species’ charge state, making it significantly clearer than existing MS analysis. In subsequent tests, all the charged particles are electrostatically removed from the beam, and unlike TOF-MS, NEMS-MS can still measure masses. This demonstrates the possibility to measure mass spectra for neutral particles. Thus, it is possible to envisage MS-based studies of analytes that are incompatible with current ionization techniques and the way is now open for the development of cutting-edge system architectures with unique analytical capability.

Bifurcation topology tuning of a mixed behavior in nonlinear micromechanical resonators

We report the experimental observation of a four-bifurcation-point (or five possible amplitudes for a given frequency) behavior of electrostatically actuated micromechanical resonators, called the mixed (first hardening then softening) behavior. We also demonstrate both analytically and experimentally tuning the bifurcation topology of this behavior via an electrostatic mechanism. An analytical model allows for the qualitative as well as quantitative explanation of the experiments and serves as a simple tool for design of nonlinear micromechanical devices under high drive.

Frequency fluctuations in silicon nanoresonators

Frequency stability is key to performance of nanoresonators. This stability is thought to reach a limit with the resonator’s ability to resolve thermally-induced vibrations. Although measurements and predictions of resonator stability usually disregard fluctuations in the mechanical frequency response, these fluctuations have recently attracted considerable theoretical interest. However, their existence is very difficult to demonstrate experimentally. Here, through a literature review, we show that all studies of frequency stability report values several orders of magnitude larger than the limit imposed by thermomechanical noise. We studied a monocrystalline silicon nanoresonator at room temperature, and found a similar discrepancy. We propose a new method to show this was due to the presence of frequency fluctuations, of unexpected level. The fluctuations were not due to the instrumentation system, or to any other of the known sources investigated. These results challenge our current understanding of frequency fluctuations and call for a change in practices.

50 nm thick AlN film-based piezoelectric cantilevers for gravimetric detection

Due to low power operation, intrinsic integrability and compatibility with CMOS processing, aluminum nitride (AlN) piezoelectric (PZE) microcantilevers are a very attractive paradigm for resonant gas sensing. In this paper, we theoretically investigate their ultimate limit of detection and enunciate design rules for performance optimization. The reduction of the AlN layer thickness is found to be critical. We further report the successful development and implementation in cantilever structures with a 50 nm thick active PZE AlN layer. Material characterizations demonstrate that the PZE e_(31) coefficient can remain as high as 0.8 C m^(−2). Electrically transduced frequency responses of the fabricated devices are in good agreement with analytical predictions. Finally, we demonstrate the excellent frequency stability with a 10^(−8) minimum Allan deviation. This exceptionally low noise operation allows us to expect a limit of detection as low as 53 zg µm^(−2) and demonstrate the strong potential of AlN PZE microcantilevers for high resolution gas detection.