Tensile testing of microfabricated thin films

 Mechanical properties of titanium thin films of 0.5 μm thickness and aluminum thin films of 1.0 μm thickness, microfabricated by magnetron sputtering, were measured by using a novel tensile machine. These thin films are difficult to handle because they are fragile, so the thin film specimens were fabricated by using semiconductor manufacturing technology in a silicon frame to protect them. The test section of these specimens was 300 μm in width and 1400 μm in gauge length. By gripping the thin film specimen with a new device using a micrometer, it could be mounted on the tensile machine easily. The stress-strain diagrams of both thin films were measured continuously in the atmosphere at room temperature. The experimental results indicated that the titanium thin film and the aluminum thin film had a smaller breaking elongation although they had a larger tensile strength than bulk pure titanium and bulk pure aluminum, respectively. Received: 31.10.96/Accepted: 14.11.96     

MEMS中Ni-W合金薄膜力学性能的研究

研究了柠檬酸胺-1-羟基乙烷二膦酸（HEDP）镀液体系中Ni-W的力学性能。通过紫外曝光的光刻、电铸和注塑（UV—LIGA）技术制备出微拉伸试样和单轴微拉伸测试系统进行拉伸试验。结果表明：在Ni-W薄膜试样尺寸为5μm×50μm×100μm条件下,其杨氏模量约为100．4GPa,抗拉强度为1．96GPa,应变约为3．6％。     

A new technique for measuring the mechanical properties of thinfilms

Accurate measurement of mechanical properties is very difficult for films that are only a few microns thick. Previously, these properties have been determined by indirect methods such as cantilever beam and diaphragm bulge tests. This paper presents a new technique to measure the Young's modulus of thin films in a direct manner consistent with its definition. Strain is measured by a laser-based technique that enables direct and accurate recording of strain on a thin-film specimen. Load is recorded with a 1-lb load cell, and an air bearing is used to eliminate friction in the loading system. The specimen is phosphorus-doped polysilicon that has a gage cross section of 3.5 μm thick by 600 μm wide. All 29 uniaxial tensile tests show brittle behavior, and the average values of Young's modulus and fracture strength are measured to be 170±6.7 GPa and 1.21±0.16 GPa, respectively. One fatigue test is also reported in this paper     

Effect of pulse frequency on the morphology and nanoindentation property of electroplated nickel films

This paper reports the effect of pulse current with different frequencies on the morphology and mechanical properties of nickel (Ni) films deposited by electroplating. The pulse frequency varies from 0 (DC) to 500 Hz while the duty cycle (T _on/T _off) is 1 during electroplating. The average roughness and deposition rate of Ni films decrease with the increasing frequency. The smoothest Ni surface with average roughness of 16.5 nm is achieved at the frequency of 500 Hz while the deposition rate reaches a nearly stable rate of 0.04 μm/min. The surface concentration of ions does not vary with time at a sufficiently high frequency with a long off time for ion to diffuse onto the surface. It will result in much more nuclei formed on the surface of cathode at a limited growth rate to get small grains for smooth morphology. The nanohardness of Ni film initially decreases rapidly from 3.9 to 1.18 GPa at 0 to 10 Hz, respectively, then increases to about 4.87 GPa in the range of 100–200 Hz, and decreases slowly to 4.0 GPa at 500 Hz. The stiffness of Ni films electroplated by pulse current at 100–200 Hz is higher than that by dc electroplating. The compromised Ni film with smooth morphology, good hardness and proper deposition rate is obtained at frequency of 100–200 Hz under the current density of 3 Adm⁻².     

Wafer-level mechanical characterization of silicon nitride MEMS

The mechanical and physical properties of silicon nitride thin films have been characterized, particularly for their application in load-bearing MEMS applications. Both stoichiometric (high-stress) and silicon-rich (low-stress) films deposited by LPCVD have been studied. Young's modulus, E, has been determined using conventional lateral resonators and by bulge testing of membranes, and tensile strength has been determined using a specially designed microtensile specimen. All microdevices have been fabricated using standard micromachining. We have also measured the thermal expansion coefficient of stoichiometric silicon nitride. Our best estimate of E is 325/spl plusmn/30 GPa for stoichiometric and 295/spl plusmn/30 GPa for silicon-rich silicon nitride. The average tensile strength for the stoichiometric material is 6.4/spl plusmn/0.6 GPa, while that for the silicon-rich material is 5.5/spl plusmn/0.8 GPa; the burst strength of membranes of the stoichiometric material is 7.1/spl plusmn/0.2 GPa.     

一种用于测试坡莫合金薄膜机械性能的拉伸模型

坡莫合金(Ni80Fe20)薄膜是微机电系统常用的磁性材料之一.介绍了一种用于测试其机械性能的单轴拉伸试验模型.此模型的特点是微小试件两端固定、且与加载机构集成在基片上,从而可减少操作工作量、提高对准精度.整个机构以微细加工方法制成:坡莫合金拉伸试件以光刻和电镀技术成型,其余的加载机构以湿法蚀刻制成.实验表明:使用此机构可以简单且高精度地对薄膜试件进行拉伸试验,获得多项力学性能参数,从而为MEMS器件设计和分析提供可靠的理论基础.     

Sub-micron coatings with low friction and wear for micro actuators

 This paper deals with the fabrication and characterisation of friction and wear reduced nano-films for micro actuator applications. For this investigation films of diamond-like-carbon (DLC), metal doped Me-DLC, carbon-nitride CN _x , boron-nitride BN and alumina Al₂O₃ films have been applied in the thickness range of 20–500 nm. The hardness of those coatings varied between 10 and 60 GPa. Micromechanical and microtribological properties of nano-coatings have been characterized by a modified scanning probe microscope. Besides this a novel micro tester for abrasive wear measurement of nano coatings was used. Friction of micro-contact areas was measured by use of a pin-on-disc tester. It turned out, that friction was – besides other parameters – dependent on determination method and load. Friction determined at areal DLC/DLC contact zones was generally much higher (μ_DLC 0.1) than diamond tip versus DLC (∼μ _DLC 0.06). Received: 19 June 2001/Accepted: 15 September 2001     

Filling of very deep, wide trenches by BenzoCycloButene polymer

A process for deep trench filling by BenzoCycloButene (BCB) polymer is explored. Deep trenches with 100-μm depth and different aspect ratios from 1.4 to 20 have been successfully filled by BCB. Besides, chemical mechanical polishing (CMP) of BCB is studied with the main goals of smoothing surface topography of substrate after BCB filling and removing excess BCB coating which may be necessary in some applications. Removal rate for BCB, V _RR, of about 0.24 μm/min has been achieved for hard cured BCB films using acid slurry. After CMP, the BCB layer showed a roughness of about 1.36 nm (Rq, measured by atomic force microscopy, AFM).     

Roll manufacturing of flexible microfluidic devices in thin PMMA and COC foils by embossing and lamination

Microfluidics on foil is gaining momentum due to a number of advantages of employing thin films combined with the capability of cost-effective high-volume manufacturing of devices. In this work, ultra-thin, flexible Y-microreactors with microchannels of 100 μm width and 30 μm depth were fabricated in thermoplastic polymer foils. The fluidic pattern was hot roll embossed in 125 μm thick poly-methyl-methacrylate (PMMA) and 130 μm thick cyclic-olefin-copolymer (COC) films using a dry-etched microstructured silicon wafer as a flat embossing tool in a laminator. The sealing of the channels was performed with two different techniques, one based on lamination of SU8 dry film resist (DFR) and the other one based on spin-coated poly-dimethylsiloxane (PDMS). Testing of the interconnected microreactor was carried out using two dye colorant solutions to demonstrate mixing.     

Development of AFM tensile test technique for evaluating mechanical properties of sub-micron thick DLC films

This paper describes mechanical properties of submicron thick diamond-like carbon (DLC) films used for surface modification in MEMS devices. A new compact tensile tester operating under an atomic force microscope (AFM) is developed to measure Young's modulus, Poisson's ratio and fracture strength of single crystal silicon (SCS) and DLC coated SCS (DLC/SCS) specimens. DLC films with a thickness ranging from 0.11 /spl mu/m to 0.58 /spl mu/m are deposited on 19-/spl mu/m-thick SCS substrate by plasma-enhanced chemical vapor deposition using a hot cathode penning ionization gauge discharge. Young's moduli of the DLC films deposited at bias voltages of -100 V and -300 V are found to be constant at 102 GPa and 121 GPa, respectively, regardless of film thickness. Poisson's ratio of DLC film is also independent of film thickness, whereas fracture strength of DLC/SCS specimens is inversely proportional to thickness. Raman spectroscopy analyses are performed to examine the effect of hydrogen content in DLC films on elastic properties. Raman spectra reveal that a reduction in hydrogen content in the films leads to better elastic properties. Finally, the proposed evaluation techniques are shown to be applicable to sub-micron thick DLC films by finite element analyses.     

基于鼓膜法的薄膜力学性能测试研究

采用自行研制的鼓膜实验装置,结合迈克尔逊激光干涉位移测量技术,获取薄膜的变形值与压力值之间的关系曲线,以实现薄膜试样力学性能的测试.对鼓膜法测试薄膜力学性能的现状做了评述;对实验原理以及装置设计进行论述;进行实验测量,并对实验结果进行有限元分析与仿真.对纯铝薄膜(纯度99.9％,厚为210 μm)进行鼓膜实验,测得其弹性模量E为68.3 GPa,与资料结果基本一致,说明研制的鼓膜实验装置测量薄膜力学性能方法切实可行.实验装置对于在微/纳机电系统(MEMS/NEMS)中广泛应用的薄膜材料的力学性能表征具有十分重要的意义.     

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.     

High-aspect-ratio microstructures fabricated by X-ray lithography of polymethylsilsesquioxane-based spin-on glass thick films

 In this paper, a process for 200 μm high-aspect-ratio micro-optical (HARM) structures fabricated by deep X-ray lithography (DXRL) of polymethylislesuioane-based spin-on glass (SOG) thick films is presented. The SOG material used in the whole procedures is polymethylsilsesquioxane (GR650), which is a kind of sol-gel derived material and can be cured at a reasonable low temperature (75 °C). A technique to cast thick GR650 films was established in the overall process. After consolidation, the GR650 thick films were machined to reach 200 μm uniformly. Then, as negative resists, the GR650 thick films were patterned directly by DXRL. X-ray irradiated regions can be selectively retained with high structural resolution by development in an organic solvent, such as methanol. Parameter screening was done to find minimum and maximum doses needed for patterning/cross-linking, to vary development time, and to explore different film thickness. The whole process is a novel of technique to create HARM structures based on SOG materials without using molds. This technique can be extended to considerably larger structural heights. Surface and bulk compositions of the irradiated films were measured by XPS and Fourier transform infrared spectroscopy. Surface quality by roughness testing system (WYKO RST) was investigated to fabricate the microstructure with a high-accuracy surface. Received: 31 October 2001/Accepted: 23 January 2002 This work was partially supported by NSF/LEQSF (2001-04)-RII-02 grant “Micro/Nanodevices for Physical, Chemical and biological Sensors”.     

Morphology and magnetic properties of electroplated Co-rich Co-Zn thin films

This work explores the microstructure and magnetic properties of electrodeposited Co-Zn thin films. Using pulse-reverse electroplating technique, Co-rich Co-Zn films are deposited 0.4–1.9 μm thick from aqueous sulfate-based baths at low temperature (55°C). The influence of current density (25–100 mA/cm²) and electrolyte Zn concentration (0–0.28 M) on the microstructure and magnetic properties are investigated. All of the Co-Zn films exhibit higher out-of-plane coercivity, as compared to in-plane. With increasing current density, the out-of-plane coercivity decreases from 50 to 40 kA/m (628–500 Oe). The influence of the Zn concentration in the electrolyte is more pronounced, affecting the grain size, film composition, and magnetic properties. The best magnetic properties were obtained from a bath with 0.21 M Zn and an average current density of 25 mA/cm², resulting in a Co₉₇Zn₃ composition and an out-of-plane coercivity of 92 kA/m (1,160 Oe).     

Microfabrication of thick tungsten films for use as absorbers of deep X-ray lithography masks

 We fabricated thick (5 μm) tungsten (W) film patterns by sputtering and dry etching, and realized a new deep X-ray lithography mask. The X-ray mask with 5-μm-thick W absorbers could expose about 1-mm-thick resist structures. In the deposition process of W films, the column structure of about 0.2 μm grain size, from which pattern edge roughness originates, disappeared by adding nitrogen into the sputtering gas. W film etching was carried out by reducing gas pressure and cooling the substrate (−40 °C), and a side etch width of below 0.2 μm was obtained. From the results of the pattern edge roughness and the side etch width, a pattern fabrication accuracy below ±0.5 μm was achieved. Furthermore, film stress, which induces pattern distortion, was reduced to below 50 MPa by controlling the sputtering gas pressure. The obtained mask achieved a pattern distortion below ±0.3 μm. Received: 7 July 1999/Accepted: 29 May 2000     

A directly strain measuring method for electroplated nickel micro-tensile test

In order to avoid the post-processing in micro-tensile tests, a directly strain measuring method is presented in this paper. The nickel tensile test specimen was electroplated in Watts solution under certain conditions. The measured Young’s modulus, ultimate tensile strength and elongation are 171.5 GPa, 2.18 GPa and 13.8%, respectively. By comparing these results to that obtained by the traditional method, this new approach has been proved reliable. Furthermore, the mean grain size of the nickel specimen measured by TEM images is about 160 nm with wide distribution. The XRD results show that nickel thin film in our experiment has no preferred orientation in the growth direction. The dimple rupture with small microvoids has been observed after the fracture of specimen.     

Sub-μm structured lotus surfaces manufacturing

Sub-μm structured surfaces allow modifying the behavior of polymer films or components. Especially in micro-fluidics a lotus-like characteristic is requested for many applications. Structure details with a high aspect ratio are necessary to decouple the bottom and the top of the functional layer. Unlike to stochastic methods, patterning with a LIGA-mold insert it is possible to structure surfaces very uniformly or even with controlled variations (e.g., with gradients). In this paper we present the process chain to realize polymer sub-μm structures with minimum lateral feature size of 400 nm and up to 4 μm high.     

A micro cycloid-gear system fabricated by multi-exposure LIGA technique

 In this paper, a prototype of 2 mm-diameter micro-cycloid gear system fabricated by the multi-exposure LIGA technique is presented. The gear system is composed of a casing and three vertically stacked disks and gears. Each part consists of three different levels. The first level, 40 μm high, was fabricated by UV-lithography, and the second as well as the third level, 195 μm and 250 μm high respectively, were processed by aligned deep X-ray lithography (DXL). The alignment error between two DXL-processed layers has been measured to be within ±5 μm range. As a result of the height control process, the deviation of structural height has been maintained within ±3 μm range for the UV-lithography-processed structures, and ±10 μm for the DXL-processed structures. Preliminary tests of gear assembly have been implemented with 125 μm-diameter commercially available glass fiber, and the further efforts are being carried out.     

Optical micro-paddle beam deflection measurement for electrostatic mechanical testing of nano-scale thin film application to MEMS

The authors describe their design for a paddle-like cantilever beam sample to relieve non-uniform stress distribution in beam-bending tests of the mechanical properties of thin film applications to MEMS. We added the sample to a custom-designed system equipped with an electrostatic panel and optical interferometer. The system overcomes problems associated with using nano-indentation for testing, and reduces errors tied to the amount of contact force required to bend the beam. Accurate paddle cantilever beam deflection was obtained using a four-step phase-shifting process with a Michelson interferometer. Film strain was determined using a simple force equilibrium equation. Residual stresses were measured at −41.3 MPa for 150 nm silver film, −3.2 MPa for 150 nm gold film, and −16.8 MPa for 150 nm copper film. We observed residual stresses for copper films at different thicknesses. The results indicate high tensile stress forms during the early deposition stage for thin copper film due to grain coalescence, and a decrease in stress with an increase in film thickness. In copper films with thicknesses greater than 153 nm, lattice relaxation associated with the surface mobility of metallic atoms changed residual stress from tension to compression.     

Pb-based ferroelectric thin film actuator for optical applications

Novel PZT thin film actuators for optical applications were proposed. Key issues for realizing the actuators such as PZT thin film processes, mechanical properties evaluation of thin films, and design for laminated structure were described. [1 1 1]-oriented PZT films were obtained by anneal/non-anneal sputtering process. Also for PZT dry etching, it was made clear low pressure and low temperature conditions were advantageous for high selectivity and etch rate. ECR etcher was used and etch rate of 1000 A/min and selectivity of 0.56 to photoresist mask were obtained. Young’s modulus and built-in stress of PZT film, measured by load-deflection method, were 72 GPa, −335 MPa respectively. Using these results, calculated deflection of each actuator was on the order of a few microns to 20 microns. It was confirmed that deflection of actuators would be enough for the application.