PZE-transduced Suspended Microchannel Resonators for sensing applications

This PhD thesis aims at developing a system which can measure the mechanical properties of fluidic samples in the picoliter range. The ultimate goal is the characterization of cancer cells and viscoelastic fluids (i.e. biological fluids), in order to study their mass and stiffness for diagnostic applications. The core of this project is the design, fabrication and characterization of hollow micromechanical resonators containing embedded microfluidic channels and provided with integrated piezoelectric (PZE) transduction. The measurement strategy consists in monitoring the device resonance frequency over time, while the analyte flows through the microchannel. Arrays of singly-clamped and doubly-clamped resonators are made of low stress Silicon Nitride (ls-SiNx) and vibrate in a frequency range from tens of kHz to few MHz. Microfluidic channels span 25%, 60% and 100% of the cantilever length in order to compare the resonance frequency shift induced by the same particle at different positions, along identically-designed beams. The goal is to disentangle analyte mass and stiffness contribution from the suspended microchannel resonator (SMR) mechanical response. The cross section of the suspended fluidic channel, 6 um x 10 um, is designed to measure particles in the same size range (i.e. red blood cells or circulating tumor cells). SMR energy dissipation is studied via FEM simulation, as a function of fluidic properties and geometrical dimensions. A coupled fluid-structure interaction (FSI) problem, based on linear elasticity and linearized Navier Stokes equations, is studied. The model is found well in agreement with theory and experiments presented in literature, considering the viscosity range of interest in case of biosensing application. The fabrication of transparent and PZE-transduced suspended microchannel resonators is achieved via a 6-mask process flow. 250, 500, 750 and 1000 um long singly- and doubly-clamped SMRs are fabricated. Microfluidic channels are defined via the etching of high aspect ratio-trenches through a sacrificial layer of polysilicon, and filled with ls-SiNx. Discontinuous etch apertures are defined on top of the buried fluidic network and enable channel emptying in 25 minutes via KOH etching. PZE electrodes in platinum and aluminum nitride are deposited via sputter deposition and provide independent actuation and readout of each resonator, for the first time in SMR arrays. The development of an experimental platform enables fluidic and electrical connections, as well as temperature control during devices characterization. The mechanical response of fabricated sensors is measured in air and vacuum environment, while channels are filled with air, water and Isopropyl Alcohol. PZE electrodes demonstrate efficient actuation, in the order of 1.5 nm/V for 250 um- long singly-clamped SMRs. However, PZE detected signals result very low in amplitude, thus optical detection via laser Doppler vibrometer is preferred. Frequency stability of fabricated sensors is studied in order to estimate their sensing performances and characterize their physical limitations. 250 um-long SMRs filled with DI water exhibit a frequency stability of 30 ppb at 400 ms integration time, in air. This result is in agreement with values found in literature for SMRs sensors and translates in an estimated mass sensitivity of few femtograms.

Design and Fabrication of Multilayer Piezoelectric NEMS Resonators

Muhammad Faizan

We have successfully demonstrated the fabrication of self-actuating multilayer NEMS resonators including cantilevers and double clamped beams. Resonant sensors are widely used as precision mass sensors for the detection and quantification of small concentration of analyte molecules in a gaseous solution or bacteria from biological sample which requires extremely high mass sensitivity and responsivity of the resonant sensor. Nanofabrication techniques have enabled the use of ultrathin layers for the fabrication of resonant sensors to significantly enhance sensitivity by reducing the mass of the sensor. Aluminum nitride (AIN) as an ultra-thin PZE layer has significant advantages over other transduction techniques due to its high PZE efficiency, good mechanical and thermal stability and compatibility with CMOS processing. 50nm ultra-thin layer of AIN was deposited over 25nm thin layer of platinum (Pt) in order to get well textured columnar growth of AIN crystals. AIN deposition parameters were carefully optimized to enhance piezoelectric response. The residual stress and piezoelectric properties of AIN film were studied as a function of deposition conditions. Short circuiting of electrodes was the most critical problem which was solved after implementing two different process flows. Oxide bridges were fabricated in order to avoid unwanted electrical contact between different metallic layers. At the end, suspended cantilevers and beams were suffering from bending due to high compressive stress in the active layer. Residual stress of -169.80 MPa was calculated using Stoney formula by measuring the curvature of wafer before and after the deposition of individual layers. Numerous studies have already been done on shifting of the resonance frequency due to the variations in attached mass on the surface of a resonator but there is still room for the investigation of surface stress changes on the resonance frequency. Application of surface stress induces a change in beam stiffness and dimensions which alter the resonance frequency of the cantilevers and doubly clamped beams. The motivation of this project was to carried out different experiments to study the effect of surface stress on the resonance frequency by using an active piezoelectric layer for the actuation of resonant structures. Application of voltage across PZE layer generates a longitudinal stress across the beam which leads to a shift in resonance frequency. Vibrometer was used to find the resonance frequency of the released devices.

2016

Theoretical and Experimental Study of Piezoelectric Modulated AlN Thin Films for Shear Mode BAW Resonators

Evgeny Milyutin

The use of acoustic resonators for sensors application has opened a new branch in research and applications of piezoelectric materials and devices. The first generation of such sensors is constituted by the quartz crystal microbalance (QCM) based on AT-cut mono-crystalline quartz. High sensitivities of gravimetric sensing in both air and liquids were demonstrated. Since the 1980s, when the first QCM-based sensor was demonstrated for the detection of silver in a liquid solution, many other application in chemical, bio-medical and environmental sensing were realized using the same concept. QCM's exhibit a very good thermal stability. The AT-cut quartz plate leads to the excitation of shear waves when used in parallel capacitor geometry. This is important for achieving high quality factors in the immersed operation of the sensor. A second generation of gravimetric sensors is based on surface acoustic wave (SAW) structures, working for instance with Love waves in a SiO2 layer on top of a LiTaO3 single crystal. SAW devices are mainly used as RF filters in television and mobile phones. SAW sensors are a side product of the much larger telecommunication market. The evolution of thin film and MEMS technology has lead to a third generation of gravimetric sensors that is based on bulk acoustic wave (BAW) resonances in piezoelectric thin films. Again, such sensors are a side product from the large telecommunication market where such resonators are used for RF filters. With every generation, the oscillation frequency increased. While QCM's operate typically at 5 MHz, the SAW resonators work typically at a few 100 MHz, and the thin film BAW resonators (TFBAR) operate typically around 2 GHz. The increase of the frequency goes together with an increase in sensitivity, and a decrease of the thickness and mass range that can be measured. The TFBARs are in some sense miniaturized analogs of QCM's operating at much higher frequencies. They are very promising as they reach higher sensitivities. This attracted the attention of researchers, and experimental evidence of the potential of TFBARs as sensors was delivered. In addition to the higher sensitivity, the miniaturization allows for using arrays of sensors with different immobilization layers as needed for drug screening. However, the application of the same TFBARs as used in telecommunications would not allow a good performance in immersed operation. It would only be good for operation in air. The principal characteristic of TFBARs used in mobile phones is the value of the electromechanical coupling and not the resonance mode at which this coupling is achieved. But for the in-liquid operated sensors, it's rather the opposite – the mode of the resonance should be such that the surface of the resonator, which tis in contact with liquid, should move parallel to the surface (in-plane motion, or transverse motion) to minimize emission of acoustic waves into the liquid. The coupling coefficient is of secondary importance in this case. Therefore, the development of shear mode TFBARs became an interesting task that was challenged by several research groups. One of the most successful solutions is the use of c-axis inclined AlN thin films. Inclination of c-axis in a parallel plate capacitor structure enables the coupling of the electric field to the shear strain, which enables the excitation of a shear mode. Such devices were successfully applied for selective sensing of organic species, such as DNA molecules, suspended in a liquid. Even if the process of deposition of c-axis inclined AlN films doesn't require hardware modification, the quality of the process is still far from the one for deposition of (0001)AlN films used in telecommunications. So the goal of this thesis was to find a solution for the shear mode TFBAR's based on (0001)AlN films. In (0001)AlN films, the shear strain cannot be induced by the electric field produced in a parallel plate geometry as the coefficient e35 and e34 of the piezoelectric tensor are zero. But there are e15 and e24 coefficients that are not zero, meaning that in-plane electric field can be used to excite the shear waves. In the frame of this work, this concept was studied theoretically and experimentally. The in-plane electric field was generated via inter-digitated electrodes (IDE). A first device type was realized in solidly mounted resonator (SMR) design and based on uniform (0001)- oriented AlN thin films. The anti-phase of the electric field in adjacent half-periods of the IDE resulted in an anti-phase movement of the corresponding regions of the film. Finite element modeling and boundary element modeling (FEM-BEM) were carried out to clarify the kind of vibrations present in the device. A kind of shear/lingitudinal mode with elliptic motions was obtained. A device was fabricated and tested both in liquid and air. The resonance of the device was observed in the expected frequency range (1.86 GHz) and high quality factors under operations in air (Q=870) and silicon oil (Q=270) were obtained. The drop of the quality factor was explained by the up and down motion of the regions of the film located directly under the IDE electrodes. Such a motion is due to anti-phase motion of different regions of the film as mentioned above. To prevent this effect, a second device type was studied. It is again based on the use of (0001)AlN thin films, but with modulated piezoelectric properties. Having different piezoelectric properties in the regions corresponding to adjacent half-periods of IDE, breaks the mirror symmetry of the device and allows for coupling the electric field to a pure shear mode. Analytical and numerical models explaining such a device were established and evaluated. The optimal situation is found when perfect Al-polar and N-polar regions of AlN are combined. This maximizes the coupling coefficient k that is derived as being proportional to the difference of e15 coefficients. Finding a way to fabricate the AlN thin film with different piezoelectric properties was thus the next objective. Growth features to decrease the piezoelectric effect were first studied. Providing rougher regions on the otherwise smooth substrate allowed to modify locally the quality of AlN thin films. Device based on such films were fabricated and characterized. The resonance of a pure shear mode was found at the expected frequency (roughly 2GHz) when the piezoelectric effect was modulated. Devices without this modulation failed to show the resonance at the exact frequency, exactly as the theory predicted. We managed to reduce two times the d33 coefficient of the film by inducing a increased roughness to the substrate – from 5.0 pm/V, corresponding to 1.5 degree rocking curve, down to 2.4pm/V, corresponding to 7 degree of rocking curve. The final step of the thesis was the process development for the simultaneous growth of Al-polar and N-polar regions within sputter deposited (0001)AlN, in order to achieve the maximal possible "piezomodulation" effect. As the sputter deposition yielded only N-polar films, we included Al-polar films from another source as seed layers. High temperature epitaxial growth methods of GaN and AlN on Si(111) and Si(100) lead to Ga- and Al-polarities. On such films, the sputter deposited AlN copies polarity from the growth substrate. The selective polarity was then obtained by preventing the expitaxy locally through a patterned oxide layer. Wet etching tests together with PFM measurements were performed to prove the dual polarity in the sputter deposited film. Finally, the integration of this process into the process flow for device fabrication was investigated.

EPFL2011

Design and Fabrication of Multilayer Piezoelectric NEMS Resonators

Muhammad Faizan

2016

Theoretical and Experimental Study of Piezoelectric Modulated AlN Thin Films for Shear Mode BAW Resonators

Evgeny Milyutin

EPFL2011