硅基PZT压电功能结构研究

PZT压电薄（厚）膜是制备MEMS传感元件和执行元件重要的功能材料,对近年PZT薄（厚）膜在MEMS领域的研究现状进行了分析,提出了一种新型的双杯PZT/Si膜片式功能结构;采用有限元方法对双杯PZT/Si膜片进行了结构优化,得到PZT和上、下硅杯的结构优化值为DPZT: D1:D2 =0.75:1.1:1;一阶模态谐振频率为13.2KHz;以氧化、双面光刻、各向异性刻蚀,以及PZT厚膜丝网印刷等工艺技术制作了双杯硅基PZT压电厚膜膜片,该膜片具有压电驱动功能。双杯PZT/Si膜片式功能结构的MEMS技术兼容性好,对芯片内其它元件或电路的影响小,适合作为MEMS片内执行元件的驱动机构。     

Characteristics of MSM photodetector fabricated on porous In0.08Ga0.92N

In this study, nanoporous structures of In_0.08Ga_0.92N thin films were synthesized using anodic etching at various etching durations. The metal–semiconductor–metal photodetectors subsequentaly have been fabricated by depositing a high work function metal (Pt) on the thin films. Results show that the responsivity of the detector increased with increasing the etching duration to reach to the maximum value at 15 min. Moreover, the rise and recovery times of the device were investigated at 390 nm chopped light.     

Development of RF magnetron sputtering method to fabricate PZT thin film actuator

PZT piezoelectric very thin films suitable for a microactuator have been deposited onto Invar alloy substrate using a high-temperature RF magnetron sputtering technique. PZT thin films must be deposited onto conductive substrate for a monomorph or a bimorph actuator. The chemical composition and the crystalline structure of these films were measured by ESCA and XRD, respectively. The chemical composition of PZT deposited stoichiometrically was almost the same as commercially-produced bulk PZT. Crystal planes (1 1 0) and (1 1 1) of PZT perovskite structure were observed in XRD analysis. When the substrate was heated to above 600 °C, SEM revealed only a very small number of pinholes on the surface. A thin (500 nm) film actuator has been characterized by measuring the piezoelectric property using a Laser Doppler Vibrograph. It was confirmed that the piezoelectric property has a linear relationship with the grain size, which also increased with the substrate temperature. The piezoelectric property of deposited PZT thin films showed a good agreement with a quoted value of bulk PZT, when the substrates were heated to 600 °C.     

基于激光多普勒技术的PZT薄膜压电性能测试研究

应用基于激光多普勒技术的微小形变分析方法,并引入数字锁相技术,成功实现了PZT(Pb(Zr,Ti)O₃)铁电薄膜的压电性能测试。对商用压电陶瓷在小信号激励下的压电性能测试表明,数字锁相技术的引入能有效抑制系统噪声,并提高激光多普勒系统的位移检测分辨率,使其达到皮米量级。此外,研究了用溶胶-凝胶技术和溶胶-电雾化技术制备得到的PZT薄膜的电压-位移曲线和压电位移"蝴蝶线",实验结果表明:在5 V直流偏置下测得两种方法制备得到的PZT薄膜的d₃₃压电系数分别为218.7 pC/N和215.8 pC/N,相应的标准偏差分别为12.7和28.6。     

Fabricating nanostructures through a combination of nano-oxidation and wet etching on silicon wafers with different surface conditions

This study investigates the surface conditions of silicon wafers with native oxide layers (NOL) or hydrogen passivated layers (HPL) and how they influence the processes of nano-oxidation and wet etching. We also explore the combination of nano-oxidation and wet etching processes to produce nanostructures. Experimental results reveal that the surface conditions of silicon wafers have a considerable impact on the results of nano-oxidation when combined with wet etching. The height and width of oxides on NOL samples exceeded the dimensions of oxides on HPL samples, and this difference became increasingly evident with an increase in applied bias voltage. The height of oxidized nanolines on the HPL sample increased after wet etching; however, the width of the lines increased only marginally. After wet etching, the height and width of oxides on the NOL were more than two times greater than those on the HPL. Increasing the applied bias voltage during nano-oxidation on NOL samples increased both the height and width of the oxides. After wet etching however, the increase in bias voltage appeared to have little effect on the height of oxidized nanolines, but the width of oxidized lines increased. This study also discovered that the use of higher applied bias voltages on NOL samples followed by wet etching results in nanostructures with a section profile closely resembling a curved surface. The use of this technique enabled researchers to create molds in the shape of a silicon nanolens array and an elegantly shaped nanoscale complex structures mold.     

Advances in thick and thin film analysis using interferometry

The use of interferometry to measure transparent and semi-transparent films is becoming more and more important as understanding of the measurement becomes more widespread. Techniques for measurement of thick films of 1 μm or greater using interferometry have been available for some time but measurement of thin films using interferometry is a much newer technique, also the effect of films coatings on interferometry measurements in general is now becoming more widely understood. The measurement of thick and thin films using interferometry is discussed in this paper.     

Structural study of nanometer-sized iron crystallites in single crystalline iron–mgo composite films

Single crystalline composite films of iron and MgO are prepared by a simultaneous vacuum deposition technique. The structures of the composite films, especially of the iron crystallites embedded, are studied by high-resolution electron microscopy and nanometer-area electron diffraction. The α-iron (b.c.c.) crystallites of 1 nm in size are epitaxially embedded in single crystalline MgO films, the orientation being (011 )[100]_Fe/(001)[100]_Mgo and (001)[11 0]_Fe//(001)[100]_Mgo. A heat treatment of the as-grown films at 500–1,000°C brings about a phase transformation of the crystallites from α-iron to γ-iron (f.c.c.), followed by a grain growth of α-iron and finally the growth of the spinel, MgFe₂O₄. The γ-iron crystallites transformed are circular plates and have strains at the periphery to accommodate the surrounding MgO-matrix. The magnetic property of the composite films is also reported.     

Characterization of self-assembling isolated ferroelectric domains by scanning force microscopy

Lead zirconate titanate (PZT) thin films were prepared by a sol–gel process on platinized Si substrate. Their microstructure and surface morphology were characterized by XRD and Scanninn Force Microscopy. Phase transformation of the prepared PZT films from pyrochlore to ferroelectric was observed by XRD and PFM (piezoresponse force microscopy), respectively. Self-assembling nano-structured ferroelectric phases are fabricated by solution deposition technique followed by the controlling kinetics of the transformation. Complex structures of ferroelectric domains in the isolated ferroelectric phases were found in the furnace annealed PZT films in the temperature range of 400–500°C. Single ferroelectric domain structure in the isolated ferroelectric phases could be found in thinner PZT films and used to study the size effect of laterally confined ferroelectric domains.     

Dynamics of space and polarization charges of ferroelectric thin films measured by atomic force microscopy

Retention behavior and local hysteresis characteristics in Pb(Zr(0.52)Ti(0.48))O(3) (PZT) thin films on Pt electrodes have been investigated by electrostatic force microscopy (EFM). A sol-gel method is used to synthesize PZT thin films and drying conditions are carefully explored over a wide range of temperature. Decay and retention mechanisms of single-poled and reverse-poled regions of the ferroelectric thin films are explained by space charge redistribution. Trapping behavior of space charges is dependent on the nature of interface between ferroelectric thin films and bottom electrodes. Local measurement of polarization-electric field curves by EFM shows inhomogeneous space charge entrapment.     

厚度效应对Pb(Zr0.53Ti0.47)O3薄膜微结构、铁电、介电性能的影响

用改进的溶胶-凝胶法在Pt(111)/Ti/SiO₂/Si(100)衬底上制备了不同厚度的高度(111)取向的Pb(Zr_0.53Ti_0.47)O₃薄膜.运用X射线衍射(XRD)和原子力显微镜(AFM)分析了薄膜的微结构,原子力显微镜表明厚度为0.3μm和0.56μm的PZT薄膜的晶粒尺寸和表面粗糙度分别为0.2～0.3μm、2～3μm和0.92nm、34nm.0.3μm和0.56μm PZT薄膜的剩余极化(Pr)和矫顽场(Ec)分别为32.2μC/²、79.9kV/cm, 27.7μC/cm²、54.4kV/cm;在频率100KHz时,薄膜的介电常数和介电损耗分别为539、0.066,821、0.029.     

Electrostatic force microscopy study on the domain switching properties of the Pb(Zr0.2Ti0.8)O3 thin films with different crystallographic orientations for the probe-based data storage

The domain switching properties of the ferroelectric Pb(Zr_0.2Ti_0.8)O₃ (PZT) thin films with two types of crystallographic orientations were investigated by electrostatic force microscopy (EFM). The crystallographic orientations of the PZT thin films were random on the (1 1 1)Pt/MgO(1 0 0) and c-axis preferred on the (1 0 0)Pt/MgO(1 0 0), respectively. When dc bias was applied to the films for writing in micro-scale area, electrostatic force images showed that the domain switching was hard in the PZT thin films with random orientation, while the pattern could clearly be written in the PZT films with c-axis orientation. The differences in the domain switching properties of each PZT thin film were investigated in the crystallographic orientations point of view, and the domain switching dynamics were also measured by investigating the nano-sized dot switching behavior with respect to the width of the applied voltage pulse.     

Characterization of lead zirconate titanate--lanthanum ruthenate thin film structures prepared by chemical solution deposition

In this work, the results of compositional and microstructural analysis of lead zirconate titanate--lanthanum ruthenate thin film structures prepared by chemical solution deposition are discussed. The cross-section transmission electron microscope (TEM) micrographs of the La-Ru-O film deposited on a SiO2/Si substrate and annealed at 700 degrees C revealed RuO2 crystals embedded in a glassy silicate matrix. When the La-Ru-O film was deposited on a Pt/TiO2/SiO2/Si substrate, RuO2 and La4Ru6O19 crystallized after annealing at 700 degrees C. After firing at 550 degrees C randomly oriented lead zirconate titanate (PZT) thin films crystallized on the La-Ru-O/SiO2/Si substrate, while on La-Ru-O/Pt/TiO2/SiO2/Si substrates PZT thin films with (111) preferred orientation were obtained. No diffusion of the Ru atoms in the PZT film was found. Ferroelectric response of PZT thin films on these substrates is shown in comparison with the PZT film deposited directly on the Pt/TiO2/SiO2/Si substrate without a La-Ru-O layer.     

基于Lamb波的压电陶瓷/环氧树脂复合材料传感器制备及应用

风力机叶片、飞机机翼等结构均为大面积曲面板类结构,基于Lamb波的结构健康检测技术对细微损伤比较敏感,是目前最具应用前景的技术之一。传统的Lamb波传感器大都采用PZT陶瓷制成,质地脆且硬度大,不能适应于曲面结构检测。将PZT陶瓷粉末与环氧树脂复合制备了一种新型柔性0-3型压电复合材料,研究了质量比、极化电场、极化温度和极化时间等因素对压电复合材料性能参数的影响,开展了多因素正交实验来确定材料制备的最优极化工艺参数。实验研究了该压电复合材料制成的传感器对Lamb波的传感响应特性,与现有的MFC、PVDF和传统压电片等传感元件的响应特性进行了对比分析。将制备的传感器应用于翼型曲面板,利用椭圆定位方法进行损伤检测。研究结果表明,PZT陶瓷/环氧树脂压电复合材料传感器具有良好的传感响应特性,能够很好地贴合于曲面板表面,与只能部分耦合于曲面板的传统压电片相比,采集的Lamb波信号更加准确,从而为曲面板类结构健康监测提供一种新型的柔性压电传感技术。     

The Design of Boundary Film-Forming PMA Viscosity Modifiers

Previous research has shown that some viscosity modifier additives are able to adsorb from oil solution on to metal surfaces to produce thick, viscous boundary films. These films enhance lubricant film formation in slow-speed and high temperature conditions and thus produce a significant reduction in friction. This article describes a systematic study of this phenomenon, which makes use of the versatile nature of polymethacrylate (PMA) chemistry. Dispersant polymethacrylates with a range of different functionalities, molecular weights, and architectures have been synthesized using controlled radical polymerization techniques. The influence of each of these features on boundary film formation and friction has been explored using optical interferometry and friction versus speed measurement. From the results, guidelines have been developed for designing PMAs having optimal boundary lubricating and, thus, friction-reducing properties.     

A Simple Laboratory Method to Pattern Sub‐Millimeter Features of Conductive Films of Gold and Indium Tin Oxide

Abstract

A simple laboratory photolithography method for patterning 100 nm thick gold and indium tin oxide (ITO) films on glass slides with 100 µm resolution without the need of special equipment is described. During the procedure, the conductive films are coated with a commercial screen printing emulsion using a modified drill as spin‐coater, then placed in contact with a negative photomask, and exposed to a 20 W light source for 30–60 min. The excess photoresist is washed off with water, and the glass slides are baked at 210°C to produce a mechanically and chemically resistant coating. The substrates are then etched in dilute aqueous HNO₃/HCl (gold) or 6 n HCl (ITO) to remove exposed gold and ITO films. After etching, the photoresist is removed by etching with peroxosulfuric acid (gold) or scraped off with a razor blade (ITO) leaving a conductive pattern. The procedure requires between 3 and 5 h of time, depending on experience.     

Characterization and mechanical/tribological properties of nano Au-TiO2 composite thin films prepared by a sol-gel process

Nano Au-TiO₂ composite thin films on Si(1 0 0) and glass substrates were successfully prepared with a facile sol-gel process followed by sintering. The morphology and mircostructure of the films were investigated via X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and scanning electron microscopy (SEM). The Au particles, of diameter 14-22 nm depending on the sintering temperatures used, were found to be well dispersed in the TiO₂ matrix, with a small amount of the particles escaped from the film. The surfaces of the films were uniform, compact and crack-free. Hardness and elastic modulus of the films were measured by using the nanoindentation technique. Friction and wear properties were investigated by using a one-way reciprocating tribometer. It was found that the highest hardness and elastic modulus values were obtained for the films prepared with 500 °C sintering temperature. The films displayed superior antiwear and friction reduction performances in sliding against an AISI 52100 steel ball. With 5.0 mol% Au, the friction coefficient was only 0.09-0.10 and the wear life was more than 2000 sliding cycles. The friction coefficient and wear life decreased with increasing sliding speed and load. The failure mechanism of the Au-TiO₂ films was identified to be light scuffing and abrasion. Those films can be potentially applied as ultra-thin lubricating coatings.     

Use of phase imaging in atomic force microscopy for measurement of viscoelastic contrast in polymer nanocomposites and molecularly thick lubricant films

Phase contrast microscopy, using an atomic force microscope, is used to detect and quantify changes in composition across polymer nanocomposites and molecularly thick lubricated surfaces. The technique takes advantage of the contrast in viscoelastic (viscous energy dissipation) properties of the different materials across the surface. Some materials, especially polymers, are found to display viscoelastic behavior. For such materials, the strain response lags the stress by a phase angle that is characteristic of the material. In tapping (or intermittent contact) mode, phase angle contrast is found to be highly dependent on vibration amplitude and mean tip-to-sample distance (setpoint). Phase angle contrast seems to be a stronger function of viscoelastic properties at relatively high vibration amplitude and low mean tip-to-sample distance. In this regime the effects of sample deformation, and thus viscoelastic properties, are dominant. In these contrast images, low phase angle corresponds to materials with low viscoelastic properties. This technique was used to find fairly reproducible phase angle contrast for polyethylene terephthalate (PET) films with embedded ceramic particles, metal particle (MP) magnetic tape, and Si(100) with a nonuniform Z-15 lubricant film. Very little correlation is found between phase angle images and friction force images for PET films with embedded ceramic particles and MP tape; phase angle images give information that cannot be obtained from topography or friction images. A numerical vibration model verifies that viscoelastic properties are dominant for high vibration amplitude and low mean tip-to-sample distance. For these conditions, the model also verifies that low phase angle corresponds to low viscoelastic properties.     

A method for preparing cross sections of films on wear surfaces for transmission electron microscopy study

A method for preparing cross sections of surface layers which exist on bulk metal substrates for transmission electron microscopy (TEM) study is described. The surface layer or film is protected by a vacuum-deposited or sputtered coating of a suitable metal. A mask is placed over the surface and non-masked areas are subjected to ion beam etching until the substrate is exposed. A thick electroplated layer is then applied to the surface. This layer adheres well to the ion-etched substrate and seals the coated surface film against damage during the usual slicing and grinding steps which are required for the preparation from bulk materials of thin foils for TEM study. The method was developed specifically for the analysis of boundary and extreme pressure lubrication films on wear surfaces together with the near-surface region of the substrate. However, it is also applicable to the investigation of oxide, corrosion and other surface films.     

复合材料板与金属板榫槽粘接结合有限元分析

榫槽连接是航空结构中常用的一种连接形式。通过对金属板和复合材料板的榫槽粘接部位进行有限元计算，分析简单拉力作用下连接部位的应力分布以及金属板和复合材料板尺寸对最大等效应力的影响。通过比较发现，在所考察范围内榫槽长度、粘接层厚度和板宽度等因素对模型等效应力的影响并不十分显著，而两种材料板之间的相对厚度对最大等效应力影响较大，随着金属板厚度的增大，整个榫槽连接结构的最大等效应力有所减小。     

Mechanisms of oiliness additives

Ultrathin film interferometry has been used to measure the boundary film-forming behaviour of long chain, carboxylic acid oiliness additives. It has been shown that in dry conditions, these acids form very thin films of around 2–3 nm thickness. However when water is present, some acids form significantly thicker films, around 10 nm in thickness. The behaviour of these films is very similar to that previously seen with metal carboxylate additive films, including thick film collapse at high rolling speeds followed by film reformation at slow speeds. It is suggested thick films formed by long chain carboxylic acid additives result from reaction of the acids at the rolling solid surfaces in the presence of water to form deposits of insoluble iron carboxylate.