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.     

Microbridge testing on symmetrical trilayer films

In this paper, we extended the microbridge testing method to characterize the mechanical properties of symmetrical trilayer thin films. Theoretically, we analyzed the deformation of a trilayer microbridge sample with a deformable boundary condition and derived load-deflection formulas in closed-form. The slope of a load-deflection curve under small deformation gives the relationship between the bending stiffness and the residual force of a trilayer microbridge. Taking this relationship, we were able to assess simultaneously the Young's modulus of two kinds of materials composing the symmetrical trilayer film and the thickness-averaged residual stress of the film. Experimentally, we fabricated symmetrical trilayer microbridge samples of SiO/sub 2//Si/sub 3/N/sub 4//SiO/sub 2/ on 4-inch p-type (100) silicon wafers and conducted the microbridge tests with a load and displacement sensing nanoindenter system equipped with a microwedge indenter. The experimental results verified the proposed microbridge testing method. The thickness-averaged residual stress of the 1.1-/spl mu/m trilayer thin films was determined to be 8.8 MPa, while the Young's modulus of the 0.3-/spl mu/m silicon oxide layers and the Young's modulus of the 0.5-/spl mu/m silicon nitride layer were evaluated to be 31 GPa and 294 GPa, respectively.     

Process Temperature–Dependent Mechanical Properties of Polysilicon Measured Using a Novel Tensile Test Structure

A new test structure was developed to measure three major unknown mechanical parameters of deposited thin films, i.e., fracture strength, Young's modulus, and residual stress. The structure was designed to have plural specimens of a deposited thin film bridging the gap of the silicon substrate and enables the easy and efficient tensile testing of the film. It was used to measure those parameters of various polysilicon films. Polysilicon is commonly used as a structural material of microelectromechanical systems (MEMS) after being deposited at a temperature below 600 degC and annealed at a temperature around 1000 degC to remove the residual stress. On the other hand, polysilicon can be also deposited at a temperature higher than 600 degC. The three parameters of polysilicon films depend on process temperature and were evaluated using the new test structure. Concerning the strength, films deposited at 560 degC had the highest strength when annealed at 850 degC. Films deposited at 625 degC and annealed at 1050 degC were weaker than those deposited at 560 degC and annealed at 1050 degC. Young's modulus was found to behave in a similar way. The trend of the residual stress was the same as already reported, but its local evaluation was possible in combination with the tensile strength determination     

A MEMS-Based Evaluation of the Mechanical Properties of Metallic Thin Films

Characterizing the mechanical properties of metal thin films is critical for the design and fabrication of metal microelectromechanical systems and integrated circuit devices. This paper focuses on wafer-level determination of the mechanical behavior of sputtered aluminum and nickel thin films, using a variety of measurement techniques. Elastic moduli have been determined in devices fabricated with standard micromachining techniques using bulge testing of square diaphragms and lateral resonator structures. We find a Young's modulus of ~70 GPa for Al and ~200 GPa for Ni, in agreement with data for the bulk metals. Using pressurize/depressurize cycles, the load-deflection curves of the membranes have also been determined, and in conjunction with finite element simulations, were used to determine the yield strength and fracture strength of these films. Residual stresses in the films have also been investigated using wafer curvature, bulge testing, and X-ray diffraction. The merits of each measurement technique are discussed.     

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     

Fracture Properties of Silicon Carbide Thin Films by Bulge Test of Long Rectangular Membrane

This paper reports the mechanical properties and fracture behavior of silicon carbide (3C-SiC) thin films grown on silicon substrates. Using bulge testing combined with a refined load-deflection model of long rectangular membranes, which takes into account the bending stiffness and prestress of the membrane material, the Young's modulus, prestress, and fracture strength for the 3C-SiC thin films with thicknesses of 0.40 and 1.42 mum were extracted. The stress distribution in the membranes under a load was calculated analytically. The prestresses for the two films were 322 plusmn 47 and 201 plusmn 34 MPa, respectively. The thinner 3C-SiC film with a strong (111) orientation has a plane-gstrain moduli of 415 plusmn 61 GPa, whereas the thicker film with a mixture of both (111) and (110) orientations exhibited a plane-strain moduli of 329 plusmn 49 GPa. The corresponding fracture strengths for the two kinds of SiC films were 6.49 plusmn 0.88 and 3.16 plusmn 0.38 GPa, respectively. The reference stresses were computed by integrating the local stress of the membrane at the fracture over edge, surface, and volume of the specimens and were fitted with Weibull distribution function. For the 0.40-mum-thick membranes, the surface integration has a better agreement between the data and the model, implying that the surface flaws are the dominant fracture origin. For the 1.42-mum-thick membranes, the surface integration presented only a slightly better fitting quality than the other two, and therefore, it is difficult to rule out unambiguously the effects of the volume and edge flaws. [2007-0191].     

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.     

Calibration of residual stress difference of MetalMUMPs silicon nitride films

The metal multi-user MEMS processes (MetalMUMPs) provide one nickel film, two silicon nitride films and one polysilicon film for constructing various nickel MEMS devices. The two silicon nitride films are either bonded together as a bi-layered structure or they sandwich the polysilicon film to form a tri-layered structure to support nickel structures. The residual stress difference of the two silicon nitride films causes undesired deformations of suspended MetalMUMPs devices. In this paper, the residual stress difference of the two MetalMUMPs silicon nitride thin films is calibrated and the result is 169 MPa. The Young’s modulus of the MetalMUMPs nitride films is also measured, which is 209 GPa.     

Quality factors in micron- and submicron-thick cantilevers

Micromechanical cantilevers are commonly used for detection of small forces in microelectromechanical sensors (e.g., accelerometers) and in scientific instruments (e.g., atomic force microscopes). A fundamental limit to the detection of small forces is imposed by thermomechanical noise, the mechanical analog of Johnson noise, which is governed by dissipation of mechanical energy. This paper reports on measurements of the mechanical quality factor Q for arrays of silicon-nitride, polysilicon, and single-crystal silicon cantilevers. By studying the dependence of Q on cantilever material, geometry, and surface treatments, significant insight into dissipation mechanisms has been obtained. For submicron-thick cantilevers, Q is found to decrease with decreasing cantilever thickness, indicating surface loss mechanisms. For single-crystal silicon cantilevers, significant increase in room temperature Q is obtained after 700°C heat treatment in either N₂ Or forming gas. At low temperatures, silicon cantilevers exhibit a minimum in Q at approximately 135 K, possibly due to a surface-related relaxation process. Thermoelastic dissipation is not a factor for submicron-thick cantilevers, but is shown to be significant for silicon-nitride cantilevers as thin as 2.3 μm     

Wafer-Scale Manufacturing of Bulk Shape-Memory-Alloy Microactuators Based on Adhesive Bonding of Titanium–Nickel Sheets to Structured Silicon Wafers

This paper presents a concept for the wafer-scale manufacturing of microactuators based on the adhesive bonding of bulk shape-memory-alloy (SMA) sheets to silicon microstructures. Wafer-scale integration of a cold-state deformation mechanism is provided by the deposition of stressed films onto the SMA sheet. A concept for heating of the SMA by Joule heating through a resistive heater layer is presented. Critical fabrication issues were investigated, including the cold-state deformation, the bonding scheme and related stresses, and the titanium–nickel (TiNi) sheet patterning. Novel methods for the transfer stamping of adhesive and for the handling of the thin TiNi sheets were developed, based on the use of standard dicing blue tape. First demonstrator TiNi cantilevers, wafer-level adhesively bonded on a microstructured silicon substrate, were successfully fabricated and evaluated. Intrinsically stressed silicon dioxide and silicon nitride were deposited using plasma-enhanced chemical vapor deposition to deform the cantilevers in the cold state. Tip deflections for 2.5-mm-long cantilevers in cold/hot state of 250/70 and 125/28 ${rm mu}hbox{m}$ were obtained using silicon dioxide and silicon nitride, respectively. The bond strength proved to be stronger than the force created by the 2.5-mm-long TiNi cantilever and showed no degradation after more than 700 temperature cycles. The shape-memory behavior of the TiNi is maintained during the integration process.$hfill$[2009-0085]      

A novel method for determining Young’s modulus of thin films by micro-strain gauges

This work presents a novel method for in-situ determining Youngs modulus of thin films at the wafer level by using a set of compact micromachined test structures and without any extra load applied to test such structures. The test structures comprise of a pair of micro-strain gauges with known Youngs modulus and a cantilever beam made of the measured film. The method utilizes inexpensive and available optical measuring equipment. An analytical model is derived to extract the Youngs modulus of the measured film. A conventional surface-sacrificial layer micromachining technique is used to fabricate the structures. The micro strain gauges employed in the measurement are made of low-pressure chemical-vapor deposition (LPCVD) undoped polycrystalline silicon films produced by Semiconductor Research Center (SRC) and the measured film is made of PECVD silicon nitride for demonstration. The average value of the obtained Youngs modulus of PECVD silicon nitride SiN_x is 170 ± 3 GPa by using strain gauges with a residual stress of 211 ± 10 MPa.This paper was supported by the National Science Council of the ROC under grant number NSC 92–2218-E-167–004. The staff of the Semiconductor Research Center at National Chiao Tung University are also appreciated, along with Dr. R. H. Horng for providing experiments at NCHU.Chi Hsiang Pan received the B.S. degree in mechanical engineering from National Chiao Tung University in 1984, M.S. Degree in mechanical engineering from National Sun Yi Xian University in 1989, and Ph.D. in mechanical engineering from National Chiao Tung University in Taiwan, R.O.C. in 1998. He has been an associate professor of department of mechanical engineering in National Chin Yi Institute of Technology since 1998. His research interests are in microelectromechanical systems, including design, modeling and fabrication of microstructures and microactuators.     

Evaluation of plasma deposited silicon nitride thin films for microsystems technology

Plasma deposited silicon nitride thin films were deposited at temperatures between 150/spl deg/C and 300/spl deg/C. Diagnostic microstructures were fabricated from the thin films using bulk micromachining, and the strain was calculated from optical measurement of postbuckling deflection. The results indicate that the residual strain of the thin films is dominated by film-substrate thermal mismatch, with the coefficient of thermal expansion monotonically increasing with decreasing deposition temperature. Metal-insulator-metal devices of variable area were also fabricated to measure the dielectric constant, which was shown to be independent of deposition temperature. The importance of these results to microsystems technology (MST) was briefly discussed.     

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％。     

Silicon nitride cantilevers with oxidation-sharpened silicon tips for atomic force microscopy

High-resolution atomic force microscopy (AFM) of soft or fragile samples requires a cantilever with a low spring constant and a sharp tip. We have developed a novel process for making such cantilevers from silicon nitride with oxidation-sharpened silicon tips. First, we made and sharpened silicon tips on a silicon wafer. Next, we deposited a thin film of silicon nitride over the tips and etched it to define nitride cantilevers and to remove it from the tips so that they protruded through the cantilevers. Finally, we etched from the back side to release the cantilevers by removing the silicon substrate. We characterized the resulting cantilevers by imaging them with a scanning electron microscope, by measuring their thermal noise spectra, and by using them to image a test sample in contact mode. A representative cantilever had a spring constant of /spl sim/0.06 N/m, and the tip had a radius of 9.2 nm and a cone angle of 36/spl deg/ over 3 /spl mu/m of tip length. These cantilevers are capable of higher resolution imaging than commercially available nitride cantilevers with oxidation-sharpened nitride tips, and they are especially useful for imaging large vertical features.     

Measurement of Young’s modulus and residual stress of thin SiC layers for MEMS high temperature applications

Silicon carbide (SiC) is a promising material for applications in harsh environments. Standard silicon (Si) microelectromechanical systems (MEMS) are limited in operating temperature to temperatures below 130°C for electronic devices and below 600°C for mechanical devices. Due to its large bandgap SiC enables MEMS with significantly higher operating temperatures. Furthermore, SiC exhibits high chemical stability and thermal conductivity. Young’s modulus and residual stress are important mechanical properties for the design of sophisticated SiC-based MEMS devices. In particular, residual stresses are strongly dependent on the deposition conditions. Literature values for Young’s modulus range from 100 to?400?GPa, and residual stresses range from 98 to?486?MPa. In this paper we present our work on investigating Young’s modulus and residual stress of SiC films deposited on single crystal bulk silicon using bulge testing. This method is based on measurement of pressure-dependent membrane deflection. Polycrystalline as well as single crystal cubic silicon carbide samples are studied. For the samples tested, average Young’s modulus and residual stress measured are 417?GPa and 89?MPa for polycrystalline samples. For single crystal samples, the according values are 388?GPa and 217?MPa. These results compare well with literature values.     

Temperature dependant dielectric breakdown of sputter-deposited AlN thin films using a time-zero approach

In MEMS (micro electromechanical system) devices, piezoelectric aluminum nitride (AlN) thin films are commonly used as functional material for sensing and actuating purposes. Additionally, AlN features excellent dielectric properties as well as a high chemical and thermal stability, making it also a good choice for passivation purposes for microelectronic devices. With those aspects and current trends towards minimization in mind, the dielectric reliability of thin AlN films is of utmost importance for the realization of advanced device concepts. In this study, we present results on the transversal dielectric strength of 100 nm AlN thin films deposited by dc magnetron sputtering. The dielectric strength is measured using a time-zero approach, using a fast voltage ramp to stress the film up to the point of breakdown. The measurements are performed at different device temperatures. In order to achieve statistical significance, at least 12 measurements are performed for each environment parameter set and the results are analyzed using the Weibull approach. Basically, lower breakdown fields are observed with increasing temperatures up to 300 °C with a characteristic breakdown field strength E ₀ following the relationship $\sqrt {E_{0} } \propto T$ as reported in literature for similar measurements performed at silicon nitride thin films. From the intersection of this linear behavior, the Poole–Frenkel (PF) barrier height ? _B is determined to 0.54 eV, which is reasonable for AlN thin films. The slope of this relation is similar to values reported for silicon nitride thin films. This allows an estimation of the breakdown field at higher temperatures by extrapolation. Leakage current measurements show a dominant PF type conduction mechanism, verifying the applicability of $\sqrt {E_{0} } \propto T$ . No breakdown occurs in negative field direction, which is attributed to the metal–insulator–semiconductor configuration of the sample and hence, the presence of a depletion layer forming in the n-doped silicon and dominating the leakage current behavior.     

Design and batch fabrication of probes for sub-100 nm scanningthermal microscopy

A batch fabrication process has been developed for making cantilever probes for scanning thermal microscopy (SThM) with spatial resolution in the sub-100 nm range. A heat transfer model was developed to optimize the thermal design of the probes. Low thermal conductivity silicon dioxide and silicon nitride were chosen for fabricating the probe tips and cantilevers, respectively, in order to minimize heat loss from the sample to the probe and to improve temperature measurement accuracy and spatial resolution. An etch process was developed for making silicon dioxide tips with tip radius as small as 20 nm. A thin film thermocouple junction was fabricated at the tip end with a junction height that could be controlled in the range of 100-600 nm. These thermal probes have been used extensively for thermal imaging of micro- and nano-electronic devices with a spatial resolution of 50 nm. This paper presents measurement results of the steady state and dynamic temperature responses of the thermal probes and examines the wear characteristics of the probes     

Anelasticity and damping of thin aluminum films on silicon substrates

A new dynamic measurement system has been developed to investigate damping in thin metal films. This system includes a vacuum chamber, in which a free-standing bilayer cantilever sample is vibrated using an electrostatic force, and a laser interferometer to measure the displacement and velocity of the sample. With this equipment, internal friction as low as 10/sup -5/ in micrometer thick metal films in a temperature range from 300 to 750 K can be measured. Free-standing cantilevers with different frequencies have been fabricated using well-established integrated circuit (IC) fabrication processes. The cantilevers consist of thin metal films on thicker Si substrates, which exhibit low damping. From measurements of internal friction of Al thin films at various temperatures and frequencies, it is possible to study relaxation processes associated with grain boundary diffusion. The activation energy calculated from the damping data is 0.57 eV, which is consistent with previous research. This value suggests that the mechanism of internal friction in pure Al films involves grain boundary diffusion controlled grain boundary sliding. A model to describe these damping effects has been developed. By deriving an expression for the diffusional strain rate using a two-dimensional (2-D) Coble creep model, and modifying the conventional standard linear solid model for the case of bending, it is possible to give a good account of the observed damping.     

Temperature-dependent microtensile testing of thin film materials for application to microelectromechanical system

A specially designed microtensile apparatus capable of carrying out a series of tests on microscale thin films for microelectromechanical system (MEMS) applications at room temperature and at temperature up to 400°C has been developed and tested, and is described here. Several MEMS-applicable thin films were measured with it, including thermally grown silicon dioxide, gold, and gold–vanadium. The silicon dioxide was tested at room temperature. Gold and gold–vanadium films were tested at room temperature and at 200 and 400°C. Examples of these results are presented.     

Mechanical characterization of post-buckled micro-bridge beams by micro-tensile testing

A micro-tensile testing system has been developed to measure the mechanical properties of post-buckled silicon dioxide micro-bridge beams. A kind of vernier-groove carrier is presented to improve alignment precision and repeatability of the measurement, and the stiffness coefficient of the tensile system is calibrated in situ in order to obtain the deformation of the tensile beams. Through analyzing a series of stress states in the beam over film preparation, post-buckling and unfolding of the beam, the initial residual stress in the film is obtained from the original load–displacement curves. The residual stress of 354 MPa is consistent with that calculated from the theory of finite deflection of buckled beams. Young’s modulus and tensile fracture strength are also obtained from the load–displacement curves. The measured modulus and strength are 64.6 ± 3 GPa and 332–489 MPa respectively. The measured properties of the thermal silicon dioxide film are reasonably coherent with other reports.