Etching behaviour of sputter-deposited aluminium nitride thin films in H3PO4 and KOH solutions

Aluminium nitride (AlN) reactively sputter deposited from an aluminium target is an interesting compound material due to its CMOS compatible fabrication process and its piezoelectric properties. For the implementation in micromachined sensors and actuators an appropriate patterning technique is needed to form elements made of AlN. Therefore, the influence of different sputtering conditions on the vertical etch rate of AlN thin films with a typical thickness of 600 nm is investigated in an etch mixture based on phosphoric acid. Under comparable conditions, such as temperature and concentration of the etchant, thin films with a high c-axis orientation are etched substantially slower compared to films with a low degree of (002) orientation. When a high c-axis orientation is present detailed analyses of the etched topographies reveal surface characteristics with a low porosity and hence, low roughness values. From temperature dependant etching experiments an activation energy of 800(± 30) meV is determined showing a reaction-controlled etching regime independent of sputter deposition conditions. For comparison, AlN films synthesized under the same conditions were etched in potassium hydroxide (KOH) at room temperature revealing comparable etching characteristics as a function of deposition parameters. Depending on the degree of (002) orientation the topography of the etched samples show a strong increase in surface roughness with time due to a selective etching behaviour between (002) and residual crystallographic planes.     

Selective modal excitation in coupled piezoelectric microcantilevers

We study in detail the first vibration modes of a piezoelectric resonator based on two coupled micro-cantilevers, also known as tuning-forks. A multiple electrode geometry lying on a layer of piezoelectric AlN allows the selective excitation of different modes, including in-plane modes. A complete optical characterization of the devices in the z- and also the x-direction has been performed employing a Doppler vibrometer. The measurements confirm the excitation and inhibition of different modes depending on the actuation signals distribution on the electrodes. The influence of the dimensions of the resonator on the coupling between the microcantilevers has also been studied. Quality factors above 4,300 have been measured for the first anti-phase in-plane mode.     

Fabrication and characterization of a piezoelectric micromirror using for optical data tracking of high-density storage

A micromirror actuated by three piezoelectric microcantilevers is presented for optical data tracking of high-density storage application. The microcantilevers are actuated by 2.5-μm-thick lead zirconate titanate (PZT) films which are deposited on the silicon-based substrate by a compatible sol–gel route. The X-ray diffraction result shows that the PZT film is perovskite structure and has a typical good ferroelectric loop. The quasi-static displacement of the mirror plate increases linearly with increasing the driving voltage and the tracking resolution on disk is as high as 8 nm/V. The micromirror also provides a high bandwidth of about 21 kHz, which is high enough to support the optical data tracking of future high-density storage.     

Fabrication of aluminium doped zinc oxide piezoelectric thin film on a silicon substrate for piezoelectric MEMS energy harvesters

Thin film piezoelectric materials play an essential role in micro electro mechanical system (MEMS) energy harvesting due to its low power requirement and high available energy densities. Non-ferroelectric piezoelectric materials such as ZnO and AlN are highly silicon compatible making it suitable for MEMS energy harvesters in self-powered microsystems. This work primarily describe the design, simulation and fabrication of aluminium doped zinc oxide (AZO) cantilever beam deposited on <100> silicon substrate. AZO was chosen due its high piezoelectric coupling coefficient, ease of deposition and excellent bonding with silicon substrate. Doping of ZnO with Al has improved the electrical properties, conductivity and thermal stability. The proposed design operates in transversal mode (d ₃₁ mode) which was structured as a parallel plated capacitor using Si/Al/AZO/Al layers. The highlight of this work is the successful design and fabrication of Al/AZO/Al on <100> silicon as the substrate to make the device CMOS compatible for electronic functionality integration. Design and finite element modeling was conducted using COMSOL? software to estimate the resonance frequency. RF Magnetron sputtering was chosen as the deposition method for aluminium and AZO. Material characterization was performed using X-ray diffraction and field emission scanning electron microscopy to evaluate the piezoelectric qualities, surface morphology and the cross section. The fabricated energy harvester generated 1.61?V open circuit output voltage at 7.77?MHz resonance frequency. The experimental results agreed with the simulation results. The measured output voltage is sufficient for low power wireless sensor nodes as an alternative power sources to traditional chemical batteries.     

Impact of the substrate dependent polarity distribution in c-axis oriented AlN thin films on the etching behaviour and the piezoelectric properties

In this work, the influence of substrate properties on the polarization of highly c-axis oriented aluminium nitride (AlN) thin films and as a consequence, on the piezoelectric properties and the wet-chemical etching behaviour is investigated. Therefore, 620 nm thin AlN layers are simultaneously sputter-deposited under nominal unheated substrate conditions on silicon (Si) substrates or on those covered with a sputter-deposited titanium (Ti) film. After wet-chemically etching in a phosphorous acid based solution at 80 °C different residues of AlN remain. Wet-chemical etching of AlN films deposited on Ti results in a high film porosity. In contrast, AlN layers on Si are either hardly attacked or the complete thin film is removed except some remaining conical shaped residues. Furthermore, we demonstrate a change in the measured electro-mechanical properties with changing maximum deposition temperature caused by a self-heating effect of the substrate during the AlN deposition process. The change in piezoelectric properties and the differing etching behaviour is caused by a change in polarity within the AlN layer. These domains are visualized by piezoresponse force microscopy measurements, and are in good agreement with the observed etching results. For layers with mixed polarization, the absolute values of the piezoelectric constant d ₃₃ are reduced due to the counteraction of piezoelectric domains with opposite polarization.     

Membrane microcantilever arrays fabrication with PZT thin films for nanorange movement

Lead zirconate titanate (PZT) piezoelectric thin films have been prepared by sol-gel method to fabricate microcantilever arrays for nano-actuation with potential applications in the hard disk drives. In order to solve the silicon over-etching problem, which leads to a low production yield in the microcantilever fabrication process, a new fabrication process using DRIE etching of silicon from the front side of the silicon wafer has been developed. Silicon free membrane microcantilevers with PZT thin films of 1 μm in thickness have been successfully fabricated with almost 100% yield by this new process. Annealing temperature and time are critical to the preparation of the sol-gel PZT thin film. The fabrication process of microcantilever arrays in planar structure will be presented. Key issues on the fabrication of the cantilever are the compatible etching process of PZT thin film and the compensation of thin film stress in all layers to obtain a flat multi-layer structure.     

CMOS兼容的ISFET传感器模型和测量电路研究

随着CMOS工艺的不断发展,将离子敏场效应晶体管(ISFET)传感器与CMOS技术相结合,以达到提高集成度、降低成本、减小系统尺寸、提高系统可靠性。在对与CMOS工艺兼容的ISFET传感器结构模型分析的基础上,研究了一种测量电路,它具有有利于消除体效应的影响、减少共模噪声的影响、克服温度漂移等优点。对该测量电路进行模拟仿真,得到输出电压与pH值之间的关系图,结果表明:其结果与理论模型仿真值基本吻合。     

Thin-film electro-acoustic sensors based on AlN and its alloys: possibilities and limitations

Sputter deposited aluminum nitride (AlN) thin films have played a central role for the successful development of the thin film electro-acoustic technology. The development has been primarily driven by one device—the thin film bulk acoustic resonator, with its primary use for high frequency filter applications for the telecom industry. Recently, increased piezoelectric properties in AlN through the alloying with scandium nitride have been identified both experimentally and theoretically. This opens up new possibilities for the thin film electro-acoustic technology. Here expectations and discussions are presented on acoustic FBAR sensor performance when based on AlN as well as on such AlN alloys to identify possible benefits and limitations. Inhere, the distinction is made between direct and in-direct (acoustic) use of the piezoelectric effect for sensor applications. These two approaches are described and compared in view of their advantages and possibilities. Especially, the indirect (or acoustic) use is identified as interesting for its versatility and good exploitation of the thin film technology to obtain highly sensitive sensor transducers. It is pointed out that the indirect approach can well be obtained internally in the piezoelectric material structure. Original calculations are presented to support the discussion.     

CMOS: compatible wafer bonding for MEMS and wafer-level 3D integration

Wafer bonding became during past decade an important technology for MEMS manufacturing and wafer-level 3D integration applications. The increased complexity of the MEMS devices brings new challenges to the processing techniques. In MEMS manufacturing wafer bonding can be used for integration of the electronic components (e.g. CMOS circuitries) with the mechanical (e.g. resonators) or optical components (e.g. waveguides, mirrors) in a single, wafer-level process step. However, wafer bonding with CMOS wafers brings additional challenges due to very strict requirements in terms of process temperature and contamination. These challenges were identified and wafer bonding process solutions will be presented illustrated with examples.     

Design,fabrication and testing of a piezoelectric energy microgenerator

This article presents the design, fabrication and characterization of a micromachined energy harvester utilizing aluminium nitride (AlN) as a piezoelectric thin film material for energy conversion of random vibrational excitations. The harvester was designed and fabricated using silicon micromachining technology where AlN is sandwiched between two electrodes on top of a silicon cantilever beam which is terminated by a silicon seismic mass. The harvester generates electric power when subjected to mechanical vibrations. The generated electrical response of the device was experimentally evaluated at various acceleration levels. A maximum power of 34.78 μW was obtained for the device with a seismic mass of 5.6 × 5.6 mm² at an acceleration value of 2 g. Various fabricated devices were tested and evaluated in terms of the generated electrical power as well as the resonant frequency.     

Piezoelectric properties of microfabricated (K,Na)NbO3 thin films

A novel microfabrication method of lead-free piezoelectric sodium potassium niobate [(K,Na)NbO₃, KNN] thin films was proposed, and the piezoelectric characteristics of the KNN microactuators were evaluated. The KNN thin films were directly deposited on microfabricated Si microcantilevers. The transverse piezoelectric coefficient d₃₁ of the KNN films was calculated as −53.5 pm/V at 20 V_pp from the tip displacement of the microcantilevers. However, the tip displacement showed large electric-field dependence because of the extrinsic piezoelectric effect, and the intrinsic piezoelectric effect of the KNN microcantilevers was smaller than that of KNN on unprocessed thick substrates. In contrast, the extrinsic piezoelectric effect was almost independent of the microfabrication of the KNN films.     

Materials development for thin film actuators

In the development of microsystems, actuators are required which can be triggered in various different ways. The actuating principles to be used are magnetostriction, the inverse piezoelectric effect, the shape memory effect, and the bimetallic effect. The variables triggered in these cases are magnetic fields, electric fields, or temperature changes. Thin film actuators are of special interest for the development of microsystems, as they can be easily scaled down to the m-range and as their manufacturing is compatible to microsystem fabrication processes. The common property of these materials is their ability to transform electrical into mechanical energy by the effects mentioned above. Of special interest are magnetostrictive or piezoelectric materials as they allow energy transformation in both directions. These inverse effects can therefore be employed as sensoric mechanism for mechanical sensors (e.g. for stress, pressure, torque) as well. The report contains a discussion of various PVD techniques sucessfully used for producing magnetostrictive films (TbFe, TbDyFe, SmFe), piezoelectric films (PbtiO₃, ZnO, AlN), shape memory films (TiNi, TiNiPd, TiPd) and bimetallic film composites (e.g. FeNi₂₀Mn₆-FeNi₄₂). The properties of these layers are presented and compared. Possible applications and future development are outlined.     

Magnetron sputtering of piezoelectric AlN and AlScN thin films and their use in energy harvesting applications

This paper reports on the deposition of AlN and Al_XSc_1?XN films by pulse magnetron sputtering. The first part will focus on the Al_XSc_1?XN deposition process in comparison to the already established AlN process. The effect of doping AlN with Sc regarding piezoelectric and mechanical properties is presented. The films show the expected increase of piezoelectric properties as well as the softening of the material with higher Sc concentrations. Above a threshold concentration of around 40 % Sc in the Al_XSc_1?XN films, there exists a separation into two phases, an Al-rich and a Sc-rich wurtzite phase, which is shown by XRD. At Sc concentrations higher than 50 %, the films are not piezoelectric, as the films are composed primarily of the cubic ScN phase. The second main part of this paper evaluates the films for application in energy harvesting. Especially the Sc doping allows a significant increase in the energy generated in our test setup. Directly measuring the AC voltage at resonance depending on load resistance with base excitation of ±2.5 µm, 350 µW power have been generated under optimum conditions compared to 70 µW for pure AlN. For a more application oriented measuring setup, a standard and a SSHI-based (“Synchronised Switch Harvesting on Inductor”) AC/DC converter circuit have been tested. The SSHI interface showed a significant improvement to 180 % compared to the standard interface.     

Design and fabrication of PZT microcantilevers with freestanding structure

For developing freestanding piezoelectric microcantilevers with low resonant frequency, some critical mechanical considerations, especially cantilever bending, were given in this study. Two strategies, using piezoelectric thick films and adding a stress compensation layer, were calculationally analyzed for mitigating the cantilever bending, and then was applied for the fabrication of PZT freestanding microcantilevers. (100) oriented PZT thick films with the thickness of 6.93 μm were grown on the Pt/SiO₂/Si substrate by chemical solution deposition (CSD), and the SiO₂ layer with the thickness of 1.0 μm was kept under the PZT layer as a stress compensation layer of the freestanding microcantilevers. The freestanding microcantilevers fabricated with the micromachining process possessed the resonant frequency of 466.1 Hz, and demonstrated no obvious cantilever bending.     

Piezoelectric unimorph valve assembled on an LTCC substrate

In this paper a piezoelectric initially open valve was designed in low temperature co-fired ceramic (LTCC), manufactured using standard processes, and tested with integrated gas channels inside the LTCC module. Actuation of the valve was based on a piezoelectric unimorph with a diameter of 15 mm and thickness of 0.35 mm glued onto the fired LTCC substrate. Subsequently, a series of tests, including flow, displacement and switching time measurements, was carried out. Measurements of the valve revealed a flow of 143 ml/min under 1 bar pressure, leakage levels of 4%, valve displacement of 1.3 μm, and closing times less than 30 ms. Additional miniaturization and integration of an embedded valve in the LTCC will be pursued, enabling improved manufacturing as a batch process and micro- and nano-litre fluid management for various applications.     

Modelling and characterization of AlN-actuated microcantilevers vibrating in the first in-plane mode

The characterization of the first in-plane mode of aluminum nitride-actuated piezoelectric microcantilevers was carried out by using electrical and optical techniques. The top electrode of the cantilever was specifically designed to allow for an efficient electrical actuation of these in-plane modes. In order to confirm the in-plane nature of the modal vibration, the detection of the electrically induced movement was performed optically with the help of a stroboscopic microscope. In parallel, resonances were also measured electrically by means of an impedance analyzer. The quality factor and the resonant frequencies of the in-plane modes were estimated from the corresponding measurement data when applying both detection techniques. Our results show quality factor values as high as 3,000 for the first in-plane mode in air.     

FBAR-on-diaphragm type electro-acoustic resonant micro-accelerometer: a theoretical study

We presented a theoretical study of the performance of a novel FBAR-on-diaphragm sensor-head structure for the FBAR-based electro-acoustic resonant micro-accelerometer. This structure overcomes disadvantages in the FBAR-beam structure for its limited cantilever beam thickness, and deficiencies in the embedded-FBAR structure for its complex micro-fabrication process. Its elastic diaphragm is made of silicon dioxide (SiO₂)/silicon nitride (Si₃N₄) bilayer film, which is not only more susceptible to the IC compatible integration process for the Si-based microstructure and the FBAR, but also improves sensitivity and temperature stability of the BAW accelerometer. FBAR-on-diaphragm type BAW accelerometer integrates the acceleration sensing structure, i.e., the SiO₂/Si₃N₄ bilayer diaphragm and the Si proof-mass, with the AlN FBAR electro-acoustic transducer. Preliminary performance analysis on FBAR-on-diaphragm type BAW accelerometer suggests that the FBAR-on-diaphragm structure is feasible. We obtained modal frequencies of the FBAR-on-diaphragm structure and stress distribution of the diaphragm under 0–100 g acceleration loads through the finite element modal analysis and static simulation, Applying the calculated maximum stress to the piezoelectric film in FBAR for qualitative analysis, and combining the dependency of elastic coefficient on stress in the Wurtzite AlN film calculated with the first-principle method, we roughly predicted the maximum elastic coefficient variation in the Wurtzite AlN film under different acceleration load. With the help of the RF simulation software ADS, we changed the longitudinal wave velocity corresponding to the elastic constants with variant acceleration loads. By comparing the resulted resonant frequencies of the sensor head without and with different acceleration loads, we qualitatively characterized its frequency shift and sensitivity. In our study, we gave further analysis of the simulation results. It reveals that the first-order modal frequency of the SiO₂/Si₃N₄ circular diaphragm is quite far away from the higher ones, which means less cross modal coupling. It also reveals that under the acceleration load, its resonant frequency with a quite linear acceleration–frequency shift characteristic will up-shift with the sensitivity of several KHz/g.     

LTCC compatible PLZT thick-films for piezoelectric devices

The production of PLZT thick-films for piezoelectric devices prepared from perovskite-type (Pb, La)(Zr, Ti)O₃ powders is described. The powder manufacture, paste preparation and thick-film production compatible with the low temperature co-fired ceramics (LTCC) process are detailed. The maximum firing temperature of applied technology is 850 °C. Measurements of the dielectric and piezoelectric properties of the produced films are carried out. The low dielectric loss (0.022) and high d₃₃ and d₃₁ piezoelectric coefficients (85.7×10⁻¹² and −34.6×10⁻¹² m/V, respectively) of the material, together with a relatively low sintering temperature, make it suitable for various applications, e.g. ultrasonics.     

Tunable MEMS piezoelectric energy harvesting device

This work is focused on low frequency (<300 Hz) vibrations due to the fact that many industrial and commercial devices operate at those frequencies. The aim of the present work is to model by numerical simulation a Si cantilever beam with an AlN piezoelectric layer concept that tunes its resonant frequency post-processing, while reducing the separation of the first two modes of resonance in order to broaden its quality factor and, therefore, to harvest more environmental energy. This paper investigates by numerical simulation the influence of perforating sections of the Si beam has on the resonant frequencies of the cantilever. The authors have found that the distance between these modes is decreased by 30 % when 0.002 mm³ is extracted in a specific location of the initial structure. This difference between modes can be reduced above 80 % if a volume of 0.004 mm³ in a specific part of the initial design is subtracted. In these conditions, the first mode is decreased about 20 % the initial value and the second mode about 60 %.     

Characteristic studies of the piezoelectrically actuated micropump with check valve

This study presents the design and fabrication of a novel piezoelectric actuator for a micropump with check valve having the advantages of miniature size, light weight and low power consumption. The micropump is designed to have five major components, namely a piezoelectric actuator, a stainless steel chamber layer with membrane, two stainless steel channel layers with two valve seats, and a nickel check valve layer with two bridge-type check valves. A prototype of the micropump, with a size of 10 × 10 × 1.0 mm, is fabricated by precise manufacturing. The check valve layer was fabricated by nickel electroforming process on a stainless steel substrate. The chamber and the channel layer were made of the stainless steel manufactured using the lithography and etching process based on MEMS fabrication technology. The experimental results demonstrate that the flow rate of micropump accurately controlled by regulating the operating frequency and voltage. The flow rate of 1.82 ml/min and back pressure of 32 kPa are obtained when the micropump is driven with alternating sine-wave voltage of 120 Vpp at 160 Hz. The micropump proposed in this study provides a valuable contribution to the ongoing development of microfluidic systems.