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Specimen Size Effect on Tensile Strength of Surface-Micromachined Polycrystalline Silicon Thin Films
Toshiyuki Tsuchiya, Member, IEEE, Osamu Tabata, Member, IEEE, Jiro Sakata, and Yasunori Taga, Member, IEEE
Abstract A new tensile tester using an electrostatic-force grip was developed to evaluate the tensile strength and the reliability of thin-lm materials. The tester was constructed in a scanning electron microscope (SEM) chamber for in situ observation and was applied for tensile testing of polycrystalline silicon (poly-Si) thin lms with dimensions of 30300 m long, 25 m wide, and 2 m thick. It was found that the mean tensile strengths of nondoped and P-doped poly-Si are 2.02.8 and 2.02.7 GPa, respectively, depending on the length of the specimens, irrespective of the specimen width. Statistical analysis of these size effects on the tensile strength predicted that the location of the fracture origin was on the edge of the specimen, which was identied by the SEM observation of the fracture surface of the thin lms. [283] Index TermsElectrostatic-force grip, fracture surface, polysilicon, specimen size effect, tensile strength, Weibull plot.

I. INTRODUCTION

ECHANICAL strength measurement of thin lms has become indispensable for microelectromechanical devices, where thin lms are used for structural materials as well as electrical materials. The mechanical reliability of the microstructures should be conrmed in order to assure the durability against the shock and the long-term usage of these devices. Some testing methods are applied to thin-lm strength measurement, such as a membrane fracture test, by applying pressure (bulge test) [1], [2] and a cantilever beam bending test [3], [4]. These methods are easy to evaluate thin lms because the specimens can be handled without touching the thin lm. However, with these tests, thin lm will sometimes fracture at the edge of a membrane or a beam due to stress concentration, and the observed values are affected by the shape of the samples. The promising way to measure the mechanical strength of thin lms without shape effect is a uniaxial tensile test. This test is suitable for investigation of the fracture mechanism and the relationship between strength and microstructures such as grain size and surface roughness. However, it is difcult to apply the conventional tensile tester for bulk materials to thinManuscript received July 12, 1997; revised September 23, 1997. Subject Editor, H. Miura. A version of this paper was published in the Proceeding of MEMS-97, Jan. 2630, 1997, Nagoya, Japan. T. Tsuchiya, J. Sakata, and Y. Taga are with Toyota Central Research and Development Laboratories, Inc., Nagakute, Aichi, 480-1192, Japan (e-mail: tutti@mosk.tytlabs.co.jp). O. Tabata is with the Department of Mechanical Engineering, Ritsumeikan University, Shiga, Japan. Publisher Item Identier S 1057-7157(98)01301-8.

lm specimens because the mechanical grip cannot be used for thin lm. Several tensile testing methods and the measured tensile strength values for thin lms have been reported [5][8]. In order to investigate fracture properties of brittle materials such as the fracture origin location and the fracture toughness, the statistical analysis of measured strength values is needed, and many specimen for the statistical analysis have to be tested. However, these properties have not been investigated with these methods because they still seem to have the same problems as the conventional tensile tester, such as the specimen damage during handling, and the troubles on setting of tensile test. For example, Koskinen et al. used an adhesive to x the specimen to the grips [5]. This is an easy way to x the specimen to a grip, but it is difcult to release the fractured specimen and to clean up the probe for the next testing. A new grip system easy to x a specimen and to release it after measurement is needed. Therefore, we proposed a new tensile tester using an electrostatic-force grip, constructed this tester in a scanning electron microscope (SEM) chamber, and performed tensile testing of surface-micromachined polycrystalline silicon (polySi) thin lms [9]. In this study, tensile strength of many specimens with various lengths and widths are measured. Using observed tensile strengths, the statistical analysis is performed in order to clarify the fracture property of poly-Si corresponding to the location of fracture origin. The principle of new tensile testing using electrostatic-force grip and the thin-lm tensile tester are explained rst, and the statistical analysis is briey explained. Then, experimental results are shown and discussed. II. THIN-FILM TENSILE TESTER A. Principle The thin-lm tensile tester is characterized by its specimen grip system. Fig. 1 shows the concept of a tensile testing using the electrostatic-force grip. The thin-lm specimen is a cantilever beam with a large free end and is fabricated on a silicon wafer by the surface micromachining process. The free end of the specimen is xed to a probe by electrostatic force. Because electrostatic force is weak force compared with mechanical force, the grip cannot x a bulk material specimen, but can x a thin-lm specimen. The electrostatic force can be easily controlled by the applying voltage. With this grip

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Fig. 1. Schematic drawing of tensile testing using electrostatic-force grip. Fig. 3. Tensile tester for thin lm.

Fig. 4. SEM micrograph of tensile testing.

generates repulsive force to release it from the probe and attractive force to x it to the substrate [Fig. 2(d)]. In this test, the thin-lm specimen can be handled as fabricated on the silicon wafer and can be set and removed from the tester without touching it. B. Apparatus
Fig. 2. Procedure of tensile test of thin lm using electrostatic force.

system, a large number of specimens enough for statistical analysis can be tested one after another sequentially without any troubles in sample preparation during the test. Fig. 2 shows the procedure of the testing. First, the probe is moved close to the free end of a specimen [Fig. 2(a)]. By applying voltage between the specimen and the probe, electrostatic force is generated and the specimen is xed [Fig. 2(b)]. Then, tensile force is applied to the specimen until it fractures [Fig. 2(c)]. During the test, the friction force between the two surfaces in contact holds the specimen [9]. After the specimen fractured, the fractured free end can be released by applying the opposite-pole voltage between the probe and substrate. The charge remaining in the free end

The thin-lm tensile tester was constructed in an SEM chamber as shown in Fig. 3. The testing procedure is monitored with the SEM. The specimen placed on a precise stage is positioned by an SEM specimen stage, and the probe is positioned by a probe stage, which is driven by a step motor. The precise stage is placed on the SEM specimen stage, is driven by a piezoelectric actuator, and applies tensile force to a specimen. Applied tensile force is monitored with a strain gauge at the probe, and the specimen displacement on testing is monitored with a strain gauge located on the precise stage. Fig. 4 shows the SEM micrograph of the tensile testing. The probe is conductive material (Si wafer) covered with insulating lm [low-pressure chemical-vapor deposition (LPCVD) Si3 N4 ]. The free end of the specimen is 1 mm long and 0.2 mm wide so that the specimen will not slip during the test. The xed end has an aluminum pad to connect to the power supply.

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Fig. 5. Thin-lm specimen for tensile test.

PROPERTIES (a)

OF

TABLE I POLY-SI THIN FILM

(b)

(c)

Fig. 6. Fabricating process of specimen: (a) depositing lms, (b) patterning poly-Si and Al lms, and (c) sacricial etching to release poly-Si lm.

The shape of the specimen has to be considered not to cause a stress concentration at the end of the tested parts. Fig. 5 shows the design of the specimen. Both the free and xed ends are tapered off to the tested part. In this design, the stress concentration factors are calculated by the nite-element method (FEM) and that of the 2- and 5- m-wide specimens are 1.09 and 1.04, respectively. III. EXPERIMENT A. Film Deposition and Specimen Preparation The lm that we have tested is poly-Si lm crystallized from amorphous lm. The crystallized poly-Si lm has the following advantages. First, the internal stress is tensile, which is suitable for micromachined applications. Second, the grain size can be controlled by the annealing temperature. The crystallization occurs above 600 C, and the grain size becomes small with increasing the annealing temperature. The specimens were fabricated with the surface micromachining process shown in Fig. 6. LPCVD amorphous silicon lm was deposited by Si2 H6 at 520 C on the substrate, where LPCVD Si3 N4 lm (thickness 0.2 m) and plasma CVDnondoped silicate glass (NSG) lm (thickness 2 m) had been deposited as an insulating layer and a sacricial layer, respectively. The amorphous lm was crystallized by annealing in nitrogen at 1000 C. Phosphorus doping was performed from POCl3 in poly-Si lm at 1000 C. The grain size of the poly-Si lms was 0.3 m, irrespective of the doping. The lm was then patterned to the specimen by photolithography and reactive

ion etching (RIE), and the aluminum pad on the xed end was formed. The specimen free end has many small etching holes to shorten sacricial etching time (Fig. 6). The sacricial layer is then removed by wet etching with hydrouoric acid (HF) and dried using p-dichlorobenzene to avoid the specimen sticking to the substrate. The properties of the nondoped and P-doped poly-Si lms are shown in Table I. The internal stress and Youngs Modulus are measured with the pressuredeection technique of rectangular membrane structure [10]. B. Tensile Testing To evaluate size effects on tensile strength, specimens of various sizes are tested. The tested parts of the specimens are 2 or 5 m wide and 30, 100, or 300 m long. Many specimens enough for statistical analysis are tensile-tested. Fracture surfaces of the tested specimens are investigated with a eld-emission SEM. C. Statistical Analysis The strength of the brittle materials is governed by the largest aw in the specimens, hence, the measured strength values show scattering. To investigate the strength of the material, this scatter of the observed strength is represented by the fracture probability under the applied stress. The Weibull distribution function is usually adopted to represent the fracture probability of brittle material. When a defect that initiates a fracture exists uniformly inside the lm, the fracture probability under the applied stress is (1) is Weibull modulus, is the effective volume that where is the volume of the tested part, and is a constant. With

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(a) Fig. 7. Tensile strength of poly-Si thin lm: (a) nondoped lm and (b) P-doped lm.

(b)

these values, mean tensile strength

is (2)

where

is the Gamma function dened as follows: (3)

In this way, the strength of the brittle materials is shown by mean strength and Weibull modulus . Weibull modulus shows the scattering of the observed strength. Small value shows that the observed strength is widely scattered. Having the higher probability of the existence of a larger aw, the larger specimen has lower strength (size effect). This effect is shown by the following equation derived from (2): (4) and are the mean strengths of the specimens where whose effective volume is and , respectively. The fracture origin location can be predicted by the size effect of the tensile strength. When the defect that initiates fracture is on the surface of the specimen, is replaced with the effective surface area , and the size effect of the tensile strength is appeared on the surface area. In the same way, would be replaced with the quantity that represents the place where the fracture origin exists. To determine the location of the fracture origin, all the observed tensile strengths are tted to the Weibull distribution functions, where the effective volume is replaced by any quantities. Then, the quantity with the best tting shows the fracture origin location. In this study, tting of the observed tensile strengths to the Weibull distribution function is performed in these two waysthe Weibull plot and maximum-likelihood method. The Weibull plot is used for the observed strengths of the same size specimens to show the Weibull modulus. At the Weibull plot, all the observed tensile strength of the same size specimens

are arranged in the order of the strength, and the fracture probability of the th specimen is dened as ( : the number of the tested specimens). The fracture probability is plotted against the tensile strength. The maximum-likelihood method is used for that of all the tested specimens to predict the fracture origin. The maximum-likelihood method is better than the Weibull plot on tting because the observed strengths are tted to the function without the assumption on the fracture probability. This method uses the likelihood function that dened as follows: (5) where shown by is the Weibull probability density function

(6) and Maximum-likelihood values of Weibull modulus the constant shown by , are calculated by solving the likelihood equation so as to maximize the value of the likelihood function . The likelihood equation is dened as follows:

(7)

IV. RESULTS The specimen of the poly-Si thin lm shows brittle fracture. During the test, tensile stress is linearly increased with the displacement of the precise stage, and the stress curve against the stage displacement has no yield point until fracture.

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TENSILE STRENGTH

OF

TABLE II POLY-SI THIN FILM AGAINST

THE

SPECIMEN SIZE

(a)

(b)

Fig. 8. Measured fracture probability as function of tensile stress. The curve is tted to Weibull distribution function.

FITTING RESULT

BY THE

TABLE III MAXIMUM-LIKELIHOOD METHOD

The specimen has no necking and no plastic deformation is observed. The specimen fractures in a random position within the tested part. Table II shows the result of each size specimens together with the number of the tensile-tested specimens. In Fig. 7, the mean tensile strength and range of the observed tensile strength are plotted. The mean tensile strength of each sample is decreased with increasing the specimen length. The mean tensile strength of P-doped lm is slightly lower than the nondoped lm. Weibull moduli of nondoped and P-doped lm tted by the Weibull plot are 5.36.9 and 8.712.6, respectively. These results show that observed strengths of nondoped lm varied widely for the same specimen size. The highest strength is about twice as high as the lowest strength in the same specimen length, and the standard deviations are about 20% of the mean strength. On the other hand, the variation of observed strength of P-doped lms is smaller than that of nondoped lm. The weakest strength of the P-doped

lm is higher than that of the nondoped lm, although the mean strength is lower. In order to investigate the testing results closely, the Weibull plots of the tensile strength of nondoped lms are shown in Fig. 8. Each plotted point shows the result of each tensile test. The curves in the plots are tting curve to the Weibull distribution function. Fig. 8(a) shows the results of the specimen with different length and the same width of 5 m. The strength of the longer specimen is plotted at the left side of the shorter specimen, and the slope of the tting curve of the longer specimen is steeper than that of the shorter one. However, the different-width specimen with the same length is distributed at almost the same place [Fig. 8(b)]. A longer specimen has lower mean strength and smaller scattering, while the width of the specimen does not affect mean strength of the specimen. In order to predict the fracture origin, all the observed values of various specimen sizes are tted to the Weibull distribution functions with the maximum-likelihood method. The tting

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Fig. 9. Weibull plot normalized by the volume, surface area, and side surface area.

results are shown in Table III, where the Weibull moduli , against likelihood functions , and reliability coefcients each Weibull distribution function of various quantities are indicated. The functions with the length and side surface area have larger values of the likelihood function, and the reliability coefcients of the length or the side surface area have the largest. Therefore, the tensile strengths of the poly-Si lms

show size effect on the length or the side surface area of the specimens. These two functions have same values because all tensile tested specimen has the same thickness. V. DISCUSSION The fracture behavior indicates that the poly-Si lm is brittle material. Since it fractures in a random position within the

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(a) Fig. 10. Fracture surface of poly-Si thin lm: (a) nondoped lm and (b) P-doped lm.

(b)

tested part, the stress concentration at the ends of the specimen tested part has little effect on the strength measurement. Therefore, the measured values in this tensile testing is the exact tensile strength of the poly-Si thin lms. In the case of the nondoped lm, the mean values of the tensile strength were 2.02.8 GPa. These are comparable with the bending strength of single-crystal silicon cantilever beam [3], which is 6%8% of the theoretical strength of a single-crystal silicon [11]. If the fracture-initiated aw is inside of the specimen, the fracture is shown using the internal aw size 2 , using toughness Grifths equation

(8) and are the surface energy and Youngs modulus where of the poly-Si thin lm, respectively. The size of the aw and of bulk single2 is estimated at 3694 nm using crystal silicon [12], which is smaller than the grain size of the poly-Si thin lm. From these results, it can be concluded that poly-Si grain boundary is not too weak to fracture. Therefore, other aws, such as surface roughness or defects, should be considered as the fracture origin of poly-Si lm as well as glass. The P-doped poly-Si lm has lower strength than the nondoped lm, but the scattering of the observed tensile strength is smaller. This difference appears to be affected by doping and thickness. The doping effect on the strength would be dominant because the thickness effect may be small estimated by the length effect on the tensile strength. The deviation of the aw size in the P-doped lm is smaller than the nondoped lm. Fig. 8 shows that the strength depends only on the length, but not on the width. In addition, Table III shows that the Weibull distribution function replaced to the length or the side surface area of the specimens is best tted to the observed tensile strength. These results show the size effects of the poly-Si specimens appear on the side surface area or only on the length of the specimen, but neither the volume or the

whole surface area of the specimen. Therefore, the fracture origin of the poly-Si thin lm is located on the side surface or on the edge of the specimens. All the observed strengths of the nondoped and P-doped lm normalized on the volumes, the whole surface areas, and the side surface areas (or the specimen length) are shown in Fig. 9. When the plot is normalized on the side surface area, the plotted point is distributed around the linear line. To determine the location of the fracture origin from the size effect observation, further investigation such as the thickness effect on the strength is required. To assure the statistical analysis, the fracture surfaces of the nondoped and P-doped specimens are investigated with the FE-SEM (Fig. 10). The both fracture surfaces have radial patterns centered at the upper-right corner. Therefore, the fracture would have been initiated from the vicinity of the corner. The specimen has many small pits on the surface, which is about 50 nm in diameter. The upper-right corner of the fracture surface has a notch, which seems to be like a pit on the surface. Most of the fracture surfaces that we have been investigated show similar patterns that have notches on the upper corner, where the fracture would be initiated. The fracture origin of the poly-Si thin lm in this study is the pit on the specimen edge, which well agrees with the statistical analysis. The tensile strength of the poly-Si thin lm is as high as the bending strength of well-prepared single-crystal silicon. However, the observed tensile strength is widely scattered. In order to assure the reliability, the scattering of the observed strength should be considered. For example, when the Weibull modulus is 5.0, applied stress in the thin-lm structure has to be below 6.8% of the mean strength so that the fracture probability would be less than 10 6 . If Weibull modulus is 10.0, the applied stress becomes up to 26% of the mean strength. In order to control the reliability of the poly-Si thin lm, the reduction of the scattering of the observed strength is more effective than the increase of the mean strength. In this case, the size of the pit on the surface of the specimen

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should be controlled. The pits on the specimen surface are formed during the sacricial etching with HF, although the mechanism of the pit formation is unknown (e.g., the oxide segregation or the grain boundaries). Continuous investigation is necessary to clarify the phenomenon.

VI. CONCLUSION Fracture origin of the poly-Si thin lms has been investigated with a new tensile tester for thin lms for assuring the reliability of the MEMS devices. This tester has a grip using electrostatic force that xes the thin-lm specimen easily. The tensile strength of poly-Si lms is 2.02.8 GPa depending on the length of the specimens, but not depending on the width. With these results, statistical analysis predicted that the fracture origin is on the edge of specimen, which is identied by the experimental observation of the fracture surface. For the future, we will investigate the properties of the materials, which is represented with the fracture toughness . The relationship between the strength and the process conditions such as doping, grain size, and anneal temperature will be claried. ACKNOWLEDGMENT The authors would like to thank H. Kadoura and M. Tada for the FE-SEM observation and useful discussion. REFERENCES
[1] J. W. Beams, The Structure and Properties of Thin Films, C. A. Neugebauer, J. D. Newkirk, and D. A. Vermilyea, Eds. New York: Wiley, 1959, p. 183. [2] A. J. Grifn, Jr., F. R. Brotzen, and C. F. Dunn, Mechanical properties and microstructures of Al-1%Si thin lm metallizations, Thin Solid Films, vol. 150, pp. 237244, 1987. Schweitz, L. Tenerz, and J. Tir [3] S. Johanson, J.-A. en, Fracture testing of silicon microelements in situ in a scanning electron microscope, J. Appl. Phys., vol. 63, no. 10, pp. 47994803, May 1988. [4] T. P. Weihs, S. Hong, J. C. Bravman, and W. D. Nix, Mechanical deection of cantilever microbeams: A new technique for testing the mechanical properties of thin lms, J. Mater. Res., vol. 3, no. 5, pp. 931942, Sept./Oct. 1988. [5] J. Koskinen, J. E. Steinwall, R. Soave, and H. H. Johnson, Microtensile testing of free-standing polysilicon bers of various grain sizes, J. Micromech. Microeng., vol. 3, no. 1, pp. 1317, Mar. 1993. [6] C. T. Rosenmayer, F. R. Brotzen, and R. J. Gale, Mechanical testing of thin lms, in MRS Symp. Proc., vol. 130, 1988, pp. 7786. Schweitz, In situ tensile [7] S. Greek, F. Ericson, S. Johansson, and J.-A. strength measurement of thick-lm and thin-lm micromachined structures, in Tech. Dig. Transducers 95, Stockholm, Sweden, 1995, pp. 5659. [8] W. N. Sharpe, Jr., B. Yuan, and R. Vaidyanathan, New test structure and techniques for measurement of mechanical properties of MEMS materials, in SPIE Proc., vol. 2880, Oct. 1996, pp. 7891. [9] T. Tsuchiya, O. Tabata, J. Sakata, and Y. Taga, Tensile testing of polycrystalline silicon thin lms using electrostatic force grip, Trans. IEEJ Sens. Micromach. Soc., vol. 116-E, no. 10, pp. 441446, 1996. [10] O. Tabata, K. Kawahara, S. Sugiyama, and I. Igarashi, Mechanical property measurement of thin lms using load-deection of composite rectangular membranes, Sens. Actuators, vol. 20, pp. 135141, 1989. [11] A. Kelly, Strong Solids. Oxford, U.K.: Clarendon, 1966. [12] W. D. Kingery, H. K. Bowen, and D. R. Uhlmann, Introduction to Creamics, 2nd ed. New York: Wiley, 1976, p. 797.

Toshiyuki Tsuchiya (M96) received the M.S. degree in precision machinery engineering from the University of Tokyo, Tokyo, Japan, in 1993. He joined Toyota Central Research and Development Laboratories, Aichi, Japan. He is currently working on silicon micromachining technology, and his research interests are in thin-lm mechanical properties evaluation and surface-micromachined resonant sensors. Mr. Tsuchiya is a Member of the Institute of Electrical Engineers of Japan.

Osamu Tabata (M89) received the M.S. degree and Ph.D. degrees from the Nagoya Institute of Technology, Nagoya, Japan, in 1981 and 1993, respectively. Since 1981, he has been with the Toyota Central Research and Development Laboratories, Aichi, Japan. In 1996, he joined the Department of Mechanical Engineering, Ritsumeikan University, Shiga, Japan. He is currently engaged in the research of micro/nano process, LIGA process, thin-lm mechanical property evaluation, and MEMS. Dr. Tabata received the Science News Award for research of a monolithic pressure-ow sensor in 1987, the Presentation Paper Award for research in anisotropic etching of silicon in TMAH solutions in 1992, and the R&D 100 Award for research in the thin-lm Youngs Modulus measurement apparatus in 1993. He is a Member of the Institute of Electrical Engineers of Japan and Society of Mechanical Engineers.

Jiro Sakata received the M.S. degree in chemistry from Nagoya University, Nagoya, Japan, in 1978 and the Dr. degree in physical engineering from the University of Tokyo, Tokyo, Japan, in 1989. Since 1978, he has been working for Toyota Central Research and Development Laboratories as a Researcher on thin-lm technology. He is currently Manager of the Advanced Device Laboratory. His research interests are inorganic material science and thin-lm technology for sensors and micromachining.

Yasunori Taga (M96) received the B.Eng. degree in applied physics in 1968 and the M.Eng. degree in 1970 in applied physics, both from the Nagoya Institute of Technology, Nagoya, Japan. He received the Ph.D. degree in materials science from Osaka University, Osaka, Japan, in 1979. He is currently a Fellow and Head of the Special Research Laboratory of Toyota Central Research and Development Laboratories. The focus of his research has been the development of thin-lm process technology of sputtering to explain the complex deposition processes. Among these, the role of kinetic energy of sputtered particles on thin-lm formation and Monte Carlo simulation of trajectory of sputtered particles are included. His work also involved optical thin-lm growth by oblique deposition showing a new interface structure between a lm and substrate which is called MotohiroTaga interface in international journals. In the eld of thin-lm applications for automobiles, his research proved very successful in industrialization of thin lms for optical, semiconductor, and sensor devices. He has published more than 120 technical papers and review articles and three book chapters. He also holds more than 50 patents. Dr. Taga has been Vice President of the Chemical Sensor Society of Japan since 1997. He is a Member of the American Institute of Physics, American Vacuum Society, and Materials Research Society.