Direct growth of few-layer graphene on AlN-based resonators for high-sensitivity gravimetric biosensors.

We present the successful growth of few-layer graphene on top of AlN-based solidly mounted resonators (SMR) using a low-temperature chemical vapour deposition (CVD) process assisted by Ni catalysts, and its effective bio-functionalization with antibodies. The SMRs are manufactured on top of fully insulating AlN/SiO2 acoustic mirrors able to withstand the temperatures reached during the CVD growth of graphene (up to 650 °C). The active AlN films, purposely grown with the c-axis tilted, effectively excite shear modes displaying excellent in-liquid performance, with electromechanical coupling and quality factors of around 3% and 150, respectively, which barely vary after graphene integration. Raman spectra reveal that the as-grown graphene is composed of less than five weakly coupled layers with a low density of defects. Two functionalization protocols of the graphene are proposed. The first one, based on a covalent binding approach, starts with a low-damage O2 plasma treatment that introduces a controlled density of defects in graphene, including carboxylic groups. After that, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride/N-hydroxysuccinimide (EDC/NHS) chemistry is used to covalently bind streptavidin molecules to the surface of the sensors. The second functionalization protocol is based on the non-covalent bonding of streptavidin on hydrophobic graphene surfaces. The two protocols end with the effective bonding of biotinylated anti-IgG antibodies to the streptavidin, which leaves the surface of the devices ready for possible IgG detection.

Gravimetric sensors operating at 1.1 GHz based on inclined c-axis ZnO grown on textured Al electrodes.

Shear mode solidly mounted resonators (SMRs) are fabricated using an inclined c-axis ZnO grown on a rough Al electrode. The roughness of the Al surface is controlled by changing the substrate temperature during the deposition process to promote the growth of inclined ZnO microcrystals. The optimum substrate temperature to obtain homogeneously inclined c-axis grains in ZnO films is achieved by depositing Al at 100 °C with a surface roughness ~9.2 nm, which caused an inclination angle of ~25° of the ZnO c-axis with respect to the surface normal. Shear mode devices with quality-factors at resonance, Q r and effective electromechanical coupling factors, [Formula: see text], as high as 180 and 3.4% are respectively measured. Mass sensitivities, S m of (4.9 ± 0.1) kHz · cm2/ng and temperature coefficient of frequency (TCF) of ~-67 ppm/K are obtained using this shear mode. The performance of the devices as viscosity sensors and biosensors is demonstrated by determining the frequency shifts of water-ethanol mixtures and detection of Rabbit immunoglobin G (IgG) whole molecule (H&L) respectively.

Effects of compensating the temperature coefficient of frequency with the acoustic reflector layers on the overall performance of solidly mounted resonators.

Thin film acoustic wave resonator based devices require compensation of temperature coefficient of frequency (TCF) in many applications. This work presents the design and fabrication of temperature compensated solidly mounted resonators (SMRs). The characteristics of each material of the layered structure have an effect on the device TCF but depending on the relative position with respect to the piezoelectric material in the stack. The influence of material properties of the different layers composing the device on the TCF is discussed in detail. TCF behavior simulation is done with Mason's model and, to take into account the deterioration of overall performance due to the finite lateral size and shape of the resonator, we have used 2D and 3D finite element modelling of the resonators. The overall behavior of the device for external loads is predicted. SMRs are designed according to simulations and fabricated with different configurations to obtain TCF as near to zero as possible with an optimized response. Resonators are made by depositing Mo/AlN/Mo piezoelectric stacks on acoustic reflectors. As reflector materials, conductive W and insulating WOx films have been used as high acoustic impedance materials. SiO2 films are used as low acoustic impedance material.

Tungsten Oxide Layers of High Acoustic Impedance for Fully Insulating Acoustic Reflectors.

Gravimetric sensors based on solidly mounted resonators require fully insulating acoustic reflectors to avoid parasitics when operating in liquid media. In this work, we propose a new high-acoustic impedance material, tungsten oxide ([Formula: see text]), for acoustic reflectors. We have optimized the sputtering conditions of [Formula: see text] to obtain nonconductive layers with mass density around [Formula: see text] and acoustic velocities for the shear and the longitudinal modes up to 2700 and 4500 m/s, respectively. Compared to other conventionally used high impedance layers, [Formula: see text] films display several manufacture advantages, such as high deposition rates, great reproducibility, and good adhesion to underlying substrates. We have demonstrated the applicability of [Formula: see text] in practical shear mode bulk acoustic wave resonators that display good performance in liquid environments.

High-acoustic-impedance tantalum oxide layers for insulating acoustic reflectors.

This work describes the assessment of the acoustic properties of sputtered tantalum oxide films intended for use as high-impedance films of acoustic reflectors for solidly mounted resonators operating in the gigahertz frequency range. The films are grown by sputtering a metallic tantalum target under different oxygen and argon gas mixtures, total pressures, pulsed dc powers, and substrate biases. The structural properties of the films are assessed through infrared absorption spectroscopy and X-ray diffraction measurements. Their acoustic impedance is assessed by deriving the mass density from X-ray reflectometry measurements and the acoustic velocity from picosecond acoustic spectroscopy and the analysis of the frequency response of the test resonators.

Influence of crystal quality on the excitation and propagation of surface and bulk acoustic waves in polycrystalline AlN films.

We investigate the excitation and propagation of acoustic waves in polycrystalline aluminum nitride films along the directions parallel and normal to the c-axis. Longitudinal and transverse propagations are assessed through the frequency response of surface acoustic wave and bulk acoustic wave devices fabricated on films of different crystal qualities. The crystalline properties significantly affect the electromechanical coupling factors and acoustic properties of the piezoelectric layers. The presence of misoriented grains produces an overall decrease of the piezoelectric activity, degrading more severely the excitation and propagation of waves traveling transversally to the c-axis. It is suggested that the presence of such crystalline defects in c-axis-oriented films reduces the mechanical coherence between grains and hinders the transverse deformation of the film when the electric field is applied parallel to the surface.

DCS Tx filters using AlN resonators with iridium electrodes.

In this paper we present the design, fabrication technology, and characterization of BAW filters for the Digital Cellular System (DCS) Tx-band at 1.75 GHz. The filters are fabricated with AlN-based solidly mounted resonators (SMR) using iridium electrodes, in an attempt to increase the effective electromechanical coupling factor of the BAW devices and achieve the bandwidth requirements of DCS filters. The design and optimization of the filters is performed with a simulation tool that uses a circuit model to compute the filter frequency response. Tx filters with balanced inputs and outputs and different topologies are designed and fabricated. The experimental filter response is compared with the simulations to determine the suitability of each design. DCS bandwidth requirements are fulfilled by using Ir/AlN/Ir stacks.

Sputtered SiO2 as low acoustic impedance material for Bragg mirror fabrication in BAW resonators.

In this paper we describe the procedure to sputter low acoustic impedance SiO(2) films to be used as a low acoustic impedance layer in Bragg mirrors for BAW resonators. The composition and structure of the material are assessed through infrared absorption spectroscopy. The acoustic properties of the films (mass density and sound velocity) are assessed through X-ray reflectometry and picosecond acoustic spectroscopy. A second measurement of the sound velocity is achieved through the analysis of the longitudinal lambda/2 resonance that appears in these silicon oxide films when used as uppermost layer of an acoustic reflector placed under an AlN-based resonator.

Tailoring disorder and dimensionality: strategies for improved solid oxide fuel cell electrolytes.

Reducing the operation temperature of solid oxide fuel cells is a major challenge towards their widespread use for power generation. This has triggered an intense materials research effort involving the search for novel electrolytes with higher ionic conductivity near room temperature. Two main directions are being currently followed: the use of doping strategies for the synthesis of new bulk materials and the implementation of nanotechnology routes for the fabrication of artificial nanostructures with improved properties. In this paper, we review our recent work on solid oxide fuel cell electrolyte materials in these two directions, with special emphasis on the importance of disorder and reduced dimensionality in determining ion conductivity. Substitution of Ti for Zr in the A(2)Zr(2-) (y)Ti(y)O(7) (A = Y, Dy, and Gd) series, directly related to yttria stabilized zirconia (a common fuel cell electrolyte), allows controlling ion mobility over wide ranges. In the second scenario we describe the strong enhancement of the conductivity occurring at the interfaces of superlattices made by alternating strontium titanate and yttria stabilized zirconia ultrathin films. We conclude that cooperative effects in oxygen dynamics play a primary role in determining ion mobility of bulk and artificially nanolayered materials and should be considered in the design of new electrolytes with enhanced conductivity.

Circuital model for the analysis of the piezoelectric response of A1N films using SAW filters.

In this paper we describe a method to assess the piezoelectric response of a piezoelectric thin film deposited on a conductive substrate. It is based on analyzing the frequency response of a surface acoustic wave (SAW) filter made on the piezoelectric thin film. For this analysis, we use a circuital model that takes into account the theoretical response of the ideal filter along with all the external and internal parasitic effects that deteriorate the response. Using this model, we can obtain the electromechanical coupling factor of the piezoelectric material (k2m) with good accuracy. If parasitic effects are not considered, k2m can be underestimated by a factor of up to 20. We have tested our model using SAW filters made on A1N thin films sputtered on substrates with different conductivities. A discussion on the relation between the different circuital elements and the physical properties of the filters also is provided.

Effect of particle bombardment on the orientation and the residual stress of sputtered AlN films for SAW devices.

We present a study of the effect of particle bombardment on the preferred orientation and the residual stress of polycrystalline aluminum nitride (AlN) thin films for surface acoustic wave (SAW) applications. Films were deposited on silicon (100) substrates by radio frequency (RF) sputtering of an aluminum target in an argon and nitrogen gas mixture. The main deposition parameters were changed as follows: the total pressure from 4 mTorr to 11 mTorr, the N2 content in the gas mixture from 20% to 80%, and the substrate self-bias voltage from -10 V to -30 V. If a sufficiently high negative substrate self-bias voltage is induced, (00.2)-oriented films are obtained over the full ranges of pressure and N2 content. Such films have values of residual stress ranging from -3 GPa to +1 GPa, depending on the deposition conditions. Our results suggest that the energy of the Ar ions colliding with the substrate controls the preferred orientation of the films, whereas the directionality of the ions (for the same energy) is the main factor determining the residual stress. To demonstrate the suitability of our material for the intended application, SAW filters with good electroacoustic response have been fabricated using AlN thin films with optimized (00.2) orientation and controlled residual stress.