Micromechanical test structures have been developed for evaluating mechanical properties of thin gold films. Using micromachining techniques, gold cantilever beams of different geometry (typically 40 to 100-µm-long, 2-µm-thick and around 1-µm-wide), were fabricated. These cantilevers were resonated by electrical excitation in a scanning electron microscope (SEM) and Young's modulus, Q-factor and fatigue properties were deduced from these experiments. The longest cantilevers showed a slight upward curvature which allowed the internal stress gradient to be evaluating.

A transversal type 3.58MHz piezoelectric resonator has been fabricated using piezoelectric ZnO thin film on ELINVER (Fe-Ni-Cr-Ti ) alloy. The ZnO/ELINVER structure piezoelectric resonator has been designed to have 2 ppm temperature coefficient of frequency (TCF) per degree from -20 degrees to 80 degrees centigrade. The temperature coefficient of ELINVER alloy can be controlled to cancel the TCF of ZnO thin film by heat annealing. The ZnO thin film on ELINVER alloy shows c-axis orientation. The c-axis orientation of the ZnO thin film is strongly influenced by the surface roughness of the ELINVER alloy. The wet etching process has been adopted to shape the resonator made from ELINVER alloy substrate. The cross section of the resonator is a structure tapered about 10 degrees, created using different sized photo masks on each side of the ELINVER surface. The tapered cross section of the transversal type resonator greatly improves the frequency characteristics of the resonator. The electrical characteristics of the resonator after the improvement include a resonance frequency of 3.58MHz trimmed by a YAG laser, and resonance resistance of about 200 Ω. The temperature coefficient of frequency is about 1.5 ppm per degree at a temperature range of-20 degrees to 80 degrees centigrade.

A new class of micro-electro-mechanical systems (MEMS) for material characterization is presented. These multilayered structures are lateral resonators which allow the determination of material properties of the different materials making up the system. Of particular significance is the ability to characterize many new materials previously untestable by resonant techniques. The basic lateral resonant structures are made of a single material, usually doped polycrystalline silicon, with beams anchored to the substrate at one end and supporting a rigid mass at the other. The rigid mass has a comb-shaped region on each side for electrostatically actuating and sensing the motion. The use of this electrostatic comb drive requires that the structure be made of a material that is electrically conductive. Thus, the class of materials which is amenable to characterization by resonance techniques has been somewhat limited. Multilayer structures, tested in conjunction with these basic monolithic structures, permit properties of both the base material and the subsequent layers to be determined. Stiffness and mass density of many new materials can be obtained by comparing the behavior of multilayer structures with their single-layer counterparts. Experimental designs and the associated analytical techniques for obtaining various properties are presented.

Polysilicon films deposited by low pressure chemical deposition (LPCVD) are the most widely used structural material for microelectromechanical systems (MEMS). However, the structural properties of LPCVD polysilicon films are known to vary significantly, depending on deposition conditions as well as post-deposition processes. This paper investigates the effects of phosphorus doping and texture on Young's modulus of polysilicon films. Polysilicon films are depostied at 585°C, 605"C, and 625°C to a thickness of 2µm. Specimens with varying phosphorus doping levels are prepared by diffusion doping at various temperatures and times using both POCl3 and phosphorsilicate glass (PSG) as the source. Texture is measured using an X-ray diffractometer. Young's modulus is calculated by taking the average of the values calculated from the resonant frequencies of four-different size lateral resonators. Our results show that Young's modulus of diffusion doped polysilicon films decreases with increasing doping concentration, and increases with increasing <111> texture.

Measurements are reported on the mechanical properties of high-aspect-ratio micromechanical structures formed using a conventional 0.5-µm CMOS process. Composite structures are etched out of the CMOS dielectric, aluminum, and gate-polysilicon thin films using a post-CMOS CHF3:O2 reactive-ion etch and followed by a SF6 :O2silicon etch for release. Microstructures have a height of 5 µm and beam widths and gaps down to 1.2 µm. Properties are strongly dependent on the relative metal and dielectric content of the beams. Beams with three metal conductors and polysilicon have an effective Young's modulus of 62 GPa, residual stress of -29 MPa, and an average out-of-plane radius of curvature of 1.9 mm. Maximum Young's modulus variation is 3 GPa die-todie, and is 9 GPa between two runs. Die-to-die variation of stress and stress gradient is poor for many beam compositions, however local matching on a die is very good. Cracking is induced in a resonant fatigue structure at 620 MPa of repetitive stress after over 50 million cycles.

Surface-micromachined polysilicon lateral resonant structures were fabricated and used to determine the temperature dependence of the Young's modulus of the polysilicon. This is done by passing a dc current through the beams during resonance testing, resulting in Joule-heating. The temperatures are calibrated by increasing the dc current until the melting point of silicon is attained. The calculated Young's moduli agree well with reported values for single crystal silicon.

In addition, metal films were sputter-deposited onto the polysilicon resonators, and similar experiments performed on the composite devices to determine the temperature dependence of the modulus of the sputtered films. Ni films demonstrate a linear decrease in Young's modulus with temperature. TiNi films demonstrate two distinct modulus values with an intermediate transition region, due to the temperature-induced reversible phase transformation exhibited by TiNi.

In this paper, we describe a technique for measuring elastic and plastic properties of thin films by microbeam deflection. The test procedure is similar to a macroscopic bending test where an external load is applied to a beam and its bending measured. Silicon oxide microbeams were made by different growth, lithography and etching techniques. The beams were then deflected with a nanoindenter, while the applied load and the displacement of the beam were recorded. Young's modulus was determined from the initial linear load-displacement behavior. Some beams were notched using a focused ion beam technique and loaded until brittle fracture occurred. These measurements permit the determination of the fracture toughness of the beam materials. In order to study plastic deformation in thin Ag films, the method was extended by depositing films onto the beams and measuring the behavior of the beam/film composite. Yielding of the Ag film was seen as a deviation from the linear-elastic behavior of the beam.

We present an experimental study on a single crystal silicon (SCS) bar subjected to pure torsion using MEMS micro instruments. The bar is in the form of a pillar, anchored at one end to the silicon substrate. It is attached to a lever arm at the other end. The pillar has a minimum cross sectional area at its mid height. The cross section coincides with the (100) plane of SCS. Torsion is generated by applying two equal forces on the lever arm on either side of the pillar. Two micro instruments apply the forces. Each consists of an electrostatic actuator and a component that calibrates it. The actuator generates high force (≈ 200 µN at 50 V) and is capable of developing large displacements (≈ 10 μm). Calibration involves determination of the force generated by the actuator at an applied voltage, as well as the linear and higher order spring constants of its springs. Each microinstrument is thus calibrated independently.

With the application of forces by the two micro instruments, a torque is generated which twists the pillar. The angle of twist at different applied voltages are recorded using an angular scale. The corresponding torques are determined from the calibration parameters of the actuators. Torque is applied until the pillar fractures. Two such sample pillars, samples 1 and 2, are tested. There cross sectional areas are 1 and 2.25 µm2. We find that both the pillars behave linearly until failure. The stresses prior to fracture are evaluated based on anisotropic theory of elasticity. Samples 1 and 2 fail at shear stresses of 5.6 and 2.6 GPa respectively. The fracture surfaces seem to coincide with the (111) plane of SCS.

Some mechanical properties of thin film microelements, e.g. fracture strength, depend on the manufacturing process, the load application as well as on size and shape of the microelements. Hence, the test structures that are used to determine mechanical properties should have dimensions of the same order of magnitude as an application structure, i.e. microelements must be used to accurately characterise MEMS. The fabrication of test structures must be realised in the same process as an intended application in order to give accurate results. Microelements are easily viewed in an SEM, but to be handled and tested in situ a micromanipulator was developed. Test structures were designed as released beams fixed to the substrate at one end, with a ring at the other. A high-precision testing unit was mounted on the micromanipulator next to the test structures. In the SEM, the testing unit was manoeuvred to grip the ring of the test structure beam and a tensile test of the beam was then executed. From the test data Young's modulus and fracture strength of polysilicon and single crystalline silicon were evaluated. Relative measurement of test structures with different beam lengths enabled Young's modulus to be evaluated with an accuracy of ±5%. Young's modulus was determined to 172±7 GPa for polysilicon and 142±9 GPa for single crystalline silicon in the <100> direction. The fracture surfaces were examined and compared. Young's modulus, yield strength and fracture strength of microelements made from electroplated nickel and nickel-iron alloy were also measured. Young's modulus was evaluated to 231±12 GPa for nickel and 155±8 GPa for nickel-iron alloy composed of 72 at% nickel and 28 at% iron.

The Young's modulus and strength of polysilicon specimens manufactured in the same production run were measured in four different laboratories. Specimens subjected to in-plane bending were tested at U. C. Berkeley and at Failure Analysis Associates, and tensile measurements were made at Caltech and Johns Hopkins. All specimens were produced at the Microelectronics Center of North Carolina (MCNC).

In bending, the Young's modulus for specimens nominally 2 µm thick was measured as 174 GPa and 137 GPa; whereas in tension, a value of 132 GPa was obtained. Modulus values of 136 GPa and 142 GPa were measured in tension on specimens nominally 1.5 µm and 3.5 µm thick. Strengths of the brittle polysilicon were 2.8 and 2.7 GPa in bending and 1.3 GPa for both thicknesses in tension.

These preliminary results were presented at Symposium N - Microelectromechanical Structures for Materials Research at the Materials Research Society meeting in April 1998. This paper is a short overview of the test methods — each of which is described elsewhere — and a documentation of the results presented at that time.

Results from a finite element analysis of a cantilever beam subjected to an equi-biaxial bending moment demonstrate that the biaxial modulus E/(1-v) must be used even for narrow beams.

Sagging of suspended or laminated structures is a common problem in the processing of Low Temperature Co-Fired Ceramics (LTCC). These glass-ceramic composites are susceptible to plastic deformation upon lamination, or under the stress of body forces once the glass transition temperature of the glass binder is reached during processing. We have designed and fabricated, using the conventional methods of LTCC fabrication, meso-scale structures (ranging in size from 100 mm to 1 cm) to quantify and seek control strategies for this problem. We have implemented bridge structures and membranes to emulate most of the conventional structures encountered during packaging or sensor (actuator) device fabrication.

We have observed that when an LTCC tape with holes larger than 400 µm in diameter is laminated, the tapes above and below deform into the cavity. For smaller diameters, deformation is negligible. Bridging structures can be compensated for the potential effect of body forces by screen-printing a thick film over-layer which exert internal tensile stresses on sintering. This can often yield straight bridges. The use of fugitive phase materials, which disappear or flow during firing, is another way of supporting bridging structures. Several of these strategies have been explored, and results are presented.

This paper addresses tension-tension (R=0) low cycle fatigue behavior of thin film Al structures released from a substrate. Al beam specimens 2 µm thick, 50 µm wide and 500 µm long (gauge length) were micromachined over a window in a Si substrate. Cyclic load-displacement behavior was investigated using a multiple step test method, in which each specimen was cycled with several blocks of constant maximum displacement amplitude. Load, displacement and temperature were recorded continuously. A load drop and a corresponding stabilized state were observed for each displacement block. Monotonic tension tests to failure were also performed for comparison. Evidence of cyclic creep was observed. SEM images revealed fatigue markings on cyclically loaded specimens but not on monotonically loaded beams.

P.V.D. tungsten films deposited on silicon wafers (covered or not with a P.E.C.V.D. silicon oxide, nitride or oxynitride sublayer) were submitted to bulge and blister tests. The mechanical equilibrium and geometry of the bulged tungsten membranes is compared to various models. From this analysis, values of the residual stresses and the Young's moduli in the films are derived, and found to be consistent with previous values deduced from curvature radius measurements or other mechanical test methods, as functions of the deposition conditions. Decohesion of the films from their substrates is easily observed on the W / SiO2 / Si membranes, and the film / sublayer interfacial fracture energy is estimated about 1 J/m2. This energy increases when the sublayer is changed from SiO2 to silicon oxi-nitride and to nitride. The W / Si membranes show a much stronger adhesion than the abovementioned ones and could not be debonded before bursting.

This paper presents the study of the strength of surface micromachined diaphragms. It is found that the diaphragm strength strongly depends on the diaphragm boundary conditions. A new fabrication technique which does not change the mask and fabrication process is proposed to improve the common step-up boundary condition. Test diaphragms with diameters from 200 µm to 800 µm and three different boundary conditions have been fabricated using silicon nitride/PSG and silicon nitride/polysilicon surface micromachining processes. Experimentally, it is found that the strength of the diaphragms is significantly improved with the new boundary conditions. The application of this technique to other surface micromachined structures is also described.

Tin oxide gas sensor can detect various gases by using the conductivity changes due to adsorption and desorption processes of gaseous molecules on its surface. The reduction of the power consumption especially for batteries back-up operation, is one of the challenge for SnO2 gas sensors. We propose a new solution using a silicon oxynitride membrane (SiOxNy) to reach this objective. Thin films of SiOxNy with different compositions have been studied. Their composition, residual stress, Young modulus and mechanical strength have been evaluated. As a result, we propose an optimized silicon oxynitride membrane with a low residual stress (-50 MPa), giving above 95% fabrication yield and low power consumption (65 mW / 450°C). A new sensors generation has been successfully fabricated and its mechanical strength and thermal performances have been evaluated. Moreover, an equation is derived, which describes the variation of the Young modulus as a function of the silicon oxynitride composition.

Thin polymer layers gain importance as interlevel dielectrics in microelectronic devices. One major drawback of this class of material is instability of mechanical properties under changing climatic condition. The paper deals with evaluation of the bulge test as complementary method for investigation of humidity induced alterations of mechanical properties. It describes measurement of intrinsic as well as humidity induced stress in polymer layers. The given results agree very well with those obtained by substrate bending. Furthermore, bulge testing proved the assumption of earlier work, that change of mechanical stress is due to a humidity induced swelling process that can be described phenomenologically by expansion coefficient and a biaxial Young's modulus independent from relative humidity. Results are given and discussed for two types of polyimide.

A technique has been developed that allows the application of free-standing membranes of polymer adhesives used in microfabricated structures. The film is made free-standing by the application of the adhesive to a polymer template, followed by an adhesion step to a microfabricated substrate, and the final release of the film by the removal of the polymer template. It was found that the surface treatment used to treat the Teflon template made it adhere too strongly to the adhesive film for this application. The results show that Gel-Paks make a suitable template for the transference of polymer films over holes of at least micron size.

Two experimental techniques for quantifying MEMS-relevant material constants of piezoelectric thin films are presented. The first is an improved version of our recently developed ‘plank method.’ This technique is used to determine the product of the biaxial elastic modulus and the piezoelectric constant d31. The updated method is easier and more precise, and it utilizes the results of dynamic as well as improved static finite-element analyses. The second method is the bulge test, here emphasizing the special requirements of piezoelectric and fragile films. Results from both techniques applied to zinc oxide are presented.

The development of power MEMS, such as the Microengine being developed at MIT, requires highly stressed structures to achieve high power densities. Material strength is, therefore, a critical issue for the design of such devices. Due to the stochastic nature of the strength of brittle materials, the length scales of the test specimens should be close to those of the structure in order to avoid excessive extrapolation of the test data. In this paper, strength characterization and supporting analysis of mesoscale biaxial flexure and radiused hub flexure single crystal silicon specimens are presented. The Weibull reference strength' of planar biaxial flexure specimens was found to lie in the range 1.2 to 4.6 GPa, depending on the surface quality. The local strength at stress concentrations was obtained by testing radiused hub flexure specimens. For the case of deep reactive ion etched (DRIE) specimens, the strength at fillet radii was found to be significantly lower than that measured from planar biaxial flexure specimens due to the inferior surface quality in such regions. It was found that strength could be significantly increased by the introduction of an additional isotropic etch after the DRIE step. The test results reported herein have important implications for the development of highly stressed microfabricated structures. The sensitivity of the mechanical strength to surface processing and etching techniques must be accounted for in the design cycle, particular with regard to the selection of the appropriate fabrication route. Furthermore, in the design of highly stressed MEMS devices, it is important to account for the stochastic nature of the material strength.