Fabrication and characterization of piezoelectric micromachined ultrasonic transducers with thick composite PZT films

Ferroelectric microelectromechanical systems (MEMS) has been a growing area of research in past decades, in which ferroelectric films are combined with silicon technology for a variety of applications, such as piezo-electric micromachined ultrasonic transducers (pMUTs), which represent a new approach to ultrasound detection and generation. For ultrasound-radiating applications, thicker PZT films are preferred because generative force and response speed of the diaphragm-type transducers increase with increasing film thickness. However, integration of 4- to 20-microm thick PZT films on silicon wafer, either the deposition or the patterning, is still a bottleneck in the micromachining process. This paper reports on a diaphragm-type pMUT. A composite coating technique based on chemical solution deposition and high-energy ball milled powder has been used to fabricate thick PZT films. Micromachining of the pMUTs using such thick films has been investigated. The fabricated pMUT with crack-free PZT films up to 7-microm thick was evaluated as an ultrasonic transmitter. The generated sound pressure level of up to 120 dB indicates that the fabricated pMUT has very good ultrasound-radiating performance and, therefore, can be used to compose pMUT arrays for generating ultrasound beam with high directivity in numerous applications. The pMUT arrays also have been demonstrated.     

Piezoelectric micromachined ultrasonic transducers based on PZT thin films

This paper describes fabrication and characterization results of piezoelectric micromachined ultrasonic transducers (pMUTs) based on 2-microm-thick Pb(Zr0.53Ti0.47O3) (PZT) thin films. The applied structures are circular plates held at four bridges, thus partially unclamped. A simple analytical model for the fully clamped structure is used as a reference to optimize design parameters such as thickness relations and electrodes, and to provide approximate predictions for coupling coefficients related to previously determined thin film properties. The best coupling coefficient was achieved with a 270-microm plate and amounted to kappa2 = 5.3%. This value compares well with the calculated value based on measured small signal dielectric (epsilon = 1050) and piezoelectric (e3l,f = 15 Cm(-2)) properties of the PZT thin film at 100 kV/cm dc bias. The resonances show relatively large Q-factors, which can be partially explained by the small diameters as compared to the sound wavelength in air and in the test liquid (Fluorinert 77). A transmit-receive experiment with two quasi-identical pMUTs was performed showing significant signal transmission up to a distance of 20 cm in air and 2 cm in the test liquid.     

硅基高度择优取向PZT厚膜的制备及性能研究

应用溶胶-凝胶法成功地在以SrTiO3(STO)为模板/阻挡层Si(001)基片上制备了La-Sr-Co-O/ Pb(Zr0.5Ti0.5)O3(PZT)/La-Sr-Co-O/STO/Si异质结,PZT的厚度为0.8μm.研究了异质结的结构和性能.实验发现,PZT结晶良好、具有(001)高度择优取向以及较高的极化强度和较小的极化强度对脉冲宽度的依赖性;当外加电压为50V时,电阻率仍＞108Ω·cm.     

Fabrication and modeling of high-frequency PZT composite thick film membrane resonators

High-frequency, thickness mode resonators were fabricated using a 7 microm piezoelectric transducer (PZT) thick film that was produced using a modified composite ceramic sol-gel process. Initial studies dealt with the integration of the PZT thick film onto the substrate. Zirconium oxide (ZrO2) was selected as a diffusion barrier layer and gave good results when used in conjunction with silicon oxide (SiO2) as an etch stop layer. Using these conditions, devices were produced and the acoustic properties measured and modeled. The resonators showed a resonant frequency of about 200 MHz, an effective electromechanical coupling coefficient of 0.34, and a Q factor of 22. Modeling was based on a Mason-type model that gave good agreement between the experimental data and the simulations. The latter showed, for the PZT thick film, an electromechanical coupling coefficient of 0.35, a stiffness of 8.65 x 10(10) N x m(-2) and an e33,f piezoelectric coefficient of 9 C x m(-2).     

Microstructure characterization of sol-gel derived PZT films

The crystallization of sol-gel derived amorphous PZT films deposited on a MgO single-crystal substrate and a SiO₂ glass substrate was examined. The pyrochlore crystallites, 5 nm in size, were homogeneously nucleated in the amorphous films at 350 °C. The nucleation temperature of pyrochlore did not depend on the type of substrate. Fine pyrochlore grains were stable even during annealing at high temperatures up to 600 °C. The perovskite formation temperature was dependent on the substrate, and was about 550 °C on the MgO single-crystal substrate and about 750 °C on the SiO₂ glass substrate. The perovskite was heterogeneously nucleated preferentially at the substrate-film interface. Perovskite nucleation was more difficult at the SiO₂ glass-film interface than at the MgO single crystal-film interface. The ease of nucleation reflected the perovskite formation temperature. Perovskite crystals grew fairly rapidly, once they were nucleated in the films. In the multiple-coated films, the interface between successive layers of PZT films was a favourable nucleation site of perovskite, and the columnar perovskite grains passing through the interface were often developed.     

纳米结构PZT铁电膜的制备及其表征

采用溶胶-凝胶(sol-gel)自旋涂敷法在硅基氧化铝纳米有序孔膜版介质上(膜版孔径尺寸20～100nm,内生长金属纳米线作为底电极一部分)制备Pb(Zr0.53Ti0.47)O3(PZT)纳米结构铁电膜,并对其介电、铁电性能及微结构进行了表征。介电测量结果表明,厚度25nm的PZT铁电膜,其介电常数在低频区域(频率104Hz)从860迅速下降到100,然后保持在100左右,直至测量频率升高到106Hz。低频区域的介电常数迅速下降是由空间电荷极化所致,它与薄膜和电极之间聚集的界面空间电荷密切相关,尤其是在薄膜与Au纳米线的弯曲界面处。介电损耗在4000Hz附近出现峰值,它来源于空间电荷的共振吸收效应。电滞回线测量结果表明,厚度为100nm的PZT铁电膜,其剩余极化强度为50μC/cm2,矫顽场强为500kV/cm。剖面透射电镜(TEM)像表明PZT纳米铁电膜与底电极(金属纳米线)直接相接触,它们之间的界面呈现一定程度的弯曲。在PZT纳米铁电薄膜后退火处理后,发现部分Au金属纳米线顶端出现分枝展宽现象;而改用Pt纳米线后可有效抑制这种现象。为兼顾氧化铝纳米有序孔膜版内的金属纳米线有序分布及PZT纳米膜的结晶度,选择合适的退火温度是制备工艺中的关键因素。     

The design and characterization of micromachined air-coupledcapacitance transducers

Air-coupled capacitance transducers have been manufactured using anisotropically etched silicon backplates and commercially available dielectric films (Kapton and Mylar). The small backplate pits which result from etching, provide well ordered and highly uniform air layers between the backplate surface and thin dielectric film. Such uniformity allows the transducers to be manufactured with reproducible characteristics (a property difficult to achieve through conventional manufacturing). Impulse response studies in generation and detection, have indicated well-damped, wideband behavior, with bandwidths extending from <100 kHz to 2.3 MHz (at the -6 dB points). These bandwidths are investigated as a function of excitation pulse width, applied bias potential, and dielectric film thickness. An estimate of detection sensitivity is also provided by comparison with a calibrated laser interferometer     

Characterization of PZT thick films fabricated by micro-pen direct-writing

Lead zirconate titanate thick films have been deposited on platinum coated alumina substrates using micro-pen direct-writing technique. The viscosity, film thickness, interface, surface roughness, dielectric, and ferroelectric properties were investigated with different paste rheology, scanning speed and distance between lines. The results showed that in order to obtain good film, the viscosity values should below 10 Pa S in the writing range, and the proper writing speed should be kept at 4 mm/s, while the distance between lines should be kept as 300 μm. Comparing with the sample prepared by screen printing, the dielectric constant was increased from 710 to 750 and the dielectric loss was decreased from 0.015 to 0.012. Moreover, the two samples had similar ferroelectric properties with the remanent polarization P _r is 30 μC/cm² and the coercive field E _c is 18 kV/cm. These results mean that the Micro-pen writing is a very effective method to prepare thick films.     

Performance and characterization of new micromachined high-frequency linear arrays

A new approach for fabricating high frequency (> 20 MHz) linear array transducers, based on laser micromachining, has been developed. A 30 MHz, 64-element, 74-microm pitch, linear array design is presented. The performance of the device is demonstrated by comparing electrical and acoustic measurements with analytical, equivalent circuit, and finite-element analysis (FEA) simulations. All FEA results for array performance have been generated using one global set of material parameters. Each fabricated array has been integrated onto a flex circuit for ease of handling, and the flex has been integrated onto a custom printed circuit board test card for ease of testing. For a fully assembled array, with an acoustic lens, the center frequency was 28.7 MHz with a one-way -3 dB and -6 dB bandwidth of 59% and 83%, respectively, and a -20 dB pulse width of -99 ns. The per-element peak acoustic power, for a +/- 30 V single cycle pulse, measured at the 10 mm focal length of the lens was 590 kPa with a -6 dB directivity span of about 30 degrees. The worst-case total cross talk of the combined array and flex assembly is for nearest neighboring elements and was measured to have an average level -40 dB across the -6 dB bandwidth of the device. Any significant deviation from simulation can be explained through limitations in apparatus calibration and in device packaging.     

Fabrication and performance of high-frequency composite transducers with triangular-pillar geometry

A single-element, 40-MHz, 3-mm diameter transducer was fabricated with a geometric focus at 9 mm. The transducer was based on a piezo-composite substrate with triangular-shaped composite pillars. The 2-way bandwidth of 50% and impedance magnitude were in agreement with that predicted using finite-element modeling. A one-way radiation pattern was collected using a needle hydrophone. The one-way -3 dB beamwidth at the geometric focus was measured to be 120 mum and the -3 dB depth of field was 2.5 mm. This is in good agreement with the theoretical predictions of 112.5 mum and 2.4 mm. The triangular-pillar composite transducer was then compared with a transducer with square composite pillars with similar volume fraction of active ceramic. A 9.5 dB reduction in the amplitude of the secondary resonance was found for the triangular-pillar composite as well as a 30% gain in the 2-way pulse bandwidth. A 256-element 30-MHz linear array was fabricated as a preliminary investigation into the use of the triangular pillar as the substrate in a high-frequency linear array transducer. In vivo images were generated with both the single-element and linear-array transducers.     

Optical and microstructural characterization of sol/gel derived cerium-doped PZT thin films

Optical properties of cerium-doped PZT thin films on sapphire prepared by a sol-gel technique are investigated using both transmission and reflection spectra in the wavelength range 200 to 900 nm. The refractive index, extinction coefficient and thickness of the film are determined from the measured transmission spectra. The packing density of the film is calculated from its refractive index using the effective medium approximation (EMA), and average oscillator strength and wavelength are estimated using a Sellmeir-type dispersion equation. Absorption coefficient (α) and the band gap energy (E_g) of each film composition are also calculated. Possible correlations of microstructure and phase formation behaviour with changes in band gap energy and other optical properties are discussed. This revised version was published online in November 2006 with corrections to the Cover Date.     

基于溶胶-凝胶的两种旋涂方法制备PZT厚膜

采用溶胶-凝胶法,研究了两种在Au/Cr/SiO2/Si基底上沉积PZT(Pb(Zr0.52Ti0.48)O3)厚膜的方法.把与PZT澄清溶胶成分相同的PZT纳米粉混入澄清PZT溶胶,然后超声混合形成PZT浆料,PZT纳米粉的粒径为50～100nm.XRD分析表明两种方法得到的PZT厚膜都获得了单相钙钛矿结构.SEM结果显示两种厚膜厚度大约4μm,第一种旋涂方法制得的PZT厚膜表面粗糙,第二种旋涂方法制得的厚膜表面致密,无裂纹.在1 kHz的测试频率下,第一种和第二种厚膜的矫顽场分别为30 kV/cm和50 kV/cm,饱和极化分别为45 μC/cm2和54 μC/cm2,剩余极化分别为25μC/cm2 and 30μC/cm2.第二种厚膜有较高的直流耐压性能,在300 kV/cm的电场下,仍然保持较好的铁电性能.因而,第二种旋涂方法能够改善PZT厚膜的表面形貌和铁电性能.     

Micro-machined high-frequency (80 MHz) PZT thick film linear arrays

This paper presents the development of a micromachined high-frequency linear array using PZT piezoelectric thick films. The linear array has 32 elements with an element width of 24 μm and an element length of 4 mm. Array elements were fabricated by deep reactive ion etching of PZT thick films, which were prepared from spin-coating of PZT sol-gel composite. Detailed fabrication processes, especially PZT thick film etching conditions and a novel transferring-and-etching method, are presented and discussed. Array designs were evaluated by simulation. Experimental measurements show that the array had a center frequency of 80 MHz and a fractional bandwidth (-6 dB) of 60%. An insertion loss of -41 dB and adjacent element crosstalk of -21 dB were found at the center frequency.     

Self-separated PZT thick films with bulk-like piezoelectric and electromechanical properties

Self-separated Pb(Zr(0.52)Ti(0.48))O(3) (PZT) films were processed by a hydrothermal deposition and a rapid thermal separation method, followed by a sol-gel filling and sintering process. The films possess excellent piezoelectric and electromechanical properties close to those of bulk material. The maximum remnant polarization is over 30 μC/cm(2) and the electromechanical coupling factor (k(t)) reaches as high as 0.52. The unique microstructure characteristics of the PZT films, such as their highly dense structure, columnar grains, well-connected grain boundaries, and well-dispersed nanopores, could all contribute to the enhanced piezoelectric and electromechanical properties.     

Fabrication of PZT sol gel composite ultrasonic transducers using batch fabrication micromolding

A new micromolding technique for fabricating high-frequency (>20 MHz) ultrasound transducers has been developed. The technique combines sol gel processing with an epoxy-based, photo-resist Su-8 micromold to form miniature PZT structures. An advantage of this technique as compared to more traditional lithographic galvanforming and abforming (LIGA) processing is that the intermediate step of producing a nickel-plated mold is avoided. Instead, the PZT is formed directly using a photo-resist. The resulting structures can be fabricated with aspect ratios up to 3:1 and thicknesses up to 50 micro. We have successfully fabricated 50-micro-thick linear array elements with 23-micro-wide elements separated by 15 kerfs. A 50-micro thick, 2.5-mm diameter, five-element annular array structure with 20-micro kerfs also has been fabricated. The micromolded PZT composite has a density of 5.7-5.8 micro 0.4 g/cm3 and a thickness coupling coefficient as high as 0.32.     

Fabrication and characterization of X-ray array detectors based on polycrystalline PbI2 thick films

Polycrystalline PbI₂ thick films were grown by using close spaced vapor deposition method on glass substrate with a conducting indium–tin-oxide coating. The morphology shows a uniquely oriented film structure with hexagonal platelets accurately being upright on substrate surface. An array detector with 12 pixels was fabricated based on this structure of the thick film. It is shown that the dark current is lower than 3 nA at bias voltage below 500 V, and the dark resistivity is as high as 10¹¹ Ω cm. A mapping of dark current density of the sensitive area of the array detector exhibits a better uniformity in the central area than the fringe area. A quick photocurrent response to X-ray excitation was obtained. The photoresponse rise time about 250 μs was obtained from the detectors and the photocurrent decays in a few seconds. The values of photocurrent are higher about two orders of magnitude than the values of dark current. The distribution of photocurrent is more uniform than that of dark current in the sensitive area of the detector.     

Capacitive micromachined ultrasonic transducers with piston-shaped membranes: fabrication and experimental characterization

Capacitive micromachined ultrasonic transducers (CMUTs) featuring piston-shaped membranes (piston CMUTs) were developed to improve device performance in terms of transmission efficiency, reception sensitivity, and fractional bandwidth (FBW). A piston CMUT has a relatively flat active moving surface whose membrane motion is closer to ideal piston-type motion compared with a CMUT with uniformly thick membranes (classical CMUT). Piston CMUTs with a more uniform surface displacement profile can achieve high output pressure with a relatively small electrode separation. The improved device capacitance and gap uniformity also enhance detection sensitivity. By adding a center mass to the membrane, a large ratio of second-order resonant frequency to first-order resonant frequency was achieved. This improved the FBW. Piston CMUTs featuring membranes of different geometric shapes were designed and fabricated using wafer bonding. Fabricating piston CMUTs is a more complex process than fabricating CMUTs with uniformly thick membranes. However, no yield loss was observed. These devices achieved ~100% improvement in transduction performance (transmission and reception) over classical CMUTs. For CMUTs with square and rectangular membranes, the FBW increased from ~110% to ~150% and from ~140% to ~175%, respectively, compared with classical CMUTs. The new devices produced a maximum output pressure exceeding 1 MPa at the transducer surface. Performance optimization using geometric membrane shape configurations was the same in both piston CMUTs and classical CMUTs.     

改进的溶胶-凝胶法制备不同厚度的PZT薄膜

采用改进的溶胶-凝胶技术,在Pt(111)/Ti/SiO2/Si(100)基底上制备了不同厚度的Pb(Zr0.50Ti0.50)O3薄膜,在600℃的退火条件下获得了晶格完善的钙钛矿结构.通过前驱体溶液的差热(DTA)、热重(TGA)实验以及PZT膜加热到不同温度的物相转化分析了PZT薄膜的相结构演化过程.采用X射线衍射仪和扫描电子显微镜表征了PZT薄膜的物相和微观形貌,用HP4194A阻抗分析仪测量了薄膜的介电性能.实验结果表明,随着退火循环次数的增多,PZT(111)相含量增加;薄膜的晶粒大小不随薄膜厚度改变;薄膜晶粒呈柱状生长;薄膜的介电常数随测量频率的增加而降低,随薄膜厚度增加而增加.