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1.1.2 12 1.1.3 ...... 41 1.1.4 ##jC# ...... 42 1.2 46 1.2.1 ...... 46 1.2.2 3C# ...... 46 1.2.3 ##?# ...... 46 1.2.4 ...... 46
2. 47 2.1 47 2.1.1 47 2.1.2 48 2.1.3 66 2.1.4 #### ...... 66 2.2 ...... 68 2.2.1#%^^'#^ ...... 68 2.2.2 ^C# ...... 68 2.2.3 68 2.2.4 68 3...... 69 3.1 ...... 69 3.1.1 ...... 69 3.1.2 ...... 70 3.1.3 Wim ...... 89 3.1.5 ##30# ...... 92 3.2 93 3.2.1 ...... 93 3.2.2 30# ...... 93 3.2.3 #Wf# ...... 93 3.2.4 ...... 93
...... 94 4.1 94 4.1.1 94 4.1.2 95 4.1.3 134 4.1.4 ##3C# ...... 135 4.2#%%#-##^3C#,##f#(D#;% ...... 136 4.2.1 136 4.2.2 30# ...... 136 4.2.3 136 4.2.4 136
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Vfc„ tfc-rT ^ o-? -yy-fey^ —12, 2001 #3 4) IEC TC47 WG4 ©SMftto Mr. R Turner to®* 17 2 9 n y Ry X~?4 ^ n-=r-yytoH-9Jfffl&l70V'T®!7 —^-ya yZ£MSUt„ CtofP NEDO to - 8 - t$St<0 g 6<] ^(Digg-efc-E, Round Robin Test om&WUZs&W tit. (6) 3~« LT<7)$SttlC'DV'TSfNVD*^S:KtcE9ELTV'< ^Sasfc •5, 1.4 fciiSg: VfiStl Round Robin Test (RRT) (OStoMM i: &ofd„ RRT mtoKSWS jrfcisWf-e® rrt t>sliS$ii,, z iUct RRTXitpT##mi3%m$jT^ 4i$, KK-^fo^yylctlX t'f>tiTV'6msRRT eStiSL, #1*18*8; Ci l:r-f 4-iR*L, LT9* y, ~v'r>v*t *db\ *E%-etop*8tt. *2$ 2. mismm ■ mm, %#. #rFSro«s (i) #%*# %L (2) ^ (###. f^toR#) *L (3) #p# *L (4) (yyvt%##) L - 9 - to 44 VK1 spn Am bn 1. sgSE^lcfcl+SWftMH 1. 1 smFwifgtfxsm 1.1.1 #$t 3*6ro#a:-X:-fc5 r*y^yyg|B$tK?ij idj; 9 , Kff$ i ^ □ ymi£ 3—9 — K ; 5ISWE, 7 4" y oy yy, ISttftiWttlWi. iffll Abstract We developed On-Chip Tensile-Testing System for evaluating mechanical properties of thin film materials used in micro-electro-mechanical systems (MEMS). The followings are obtained results in the second year. (1) We surveyed the previous works which have been performed for measuring the mechanical properties of MEMS materials. (2) We developed the fabrication process of the devices having the specimen of single-crystal- and poly-silicon materials for the Round Robin Test (RRT). The specimen has several marks on the test specimen to measure the elongation during the tensile test. (3) We developed an external loading mechanism and a displacement measuring system. Load is applied using a double-cantilever spring and the elongation of the specimen is directly measured by optical images taken during the test. We tested the single-crystal silicon specimen, which is fabricated for the RRT, by using On-Chip Tensile Testing System. We obtained the results of 162 GPa of Young ’s modulus and 2.55 % of fracture elongation. 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K±e$4^b, WmL4c fftt y x x A "C# 1>*S * £ EtE SI £KK# 43-C-t 6 C t trStf&Lfco —39— % 4 : 10// m i.i.3 $stt 3*6 (ci. >) -?'(v a-?6> LTW?ESrtTV\ (1) *ffl&IHS6T?l*t>*i./'dl@S i'DTyyMJritit L/ctt*roW6 nJfigK/.toTSfcZirSrrSU ^(DijllKSfMKTto 2) Knfvfx Bt¥S, 1*6 LfctFISiii&tF^eBB-y V = ViiSg0K^>F<1 sK7'D-fey|r7 ?y Kp t" yyx ^WSlcff9 KSItff®7"n-fe7Lfc, A icliftifcfe tt®ffl 4= *w?£fiff fHiSR(f#»yo t y ros-s-ltSr 0 4 . «AN-#ID y y^ieKs^ity/w y l/c„ 3) -V:?3l»iS!gi B^S, *AL/C#SteSt>-f^SI6Sg±"1:'Ay4 :"r'yg|®M7) s"t'S d J: ) IcSB&SSr ffv\ ate5>A?|gro$6E.^ff # 6 Z Sr £r#SL/c„ (2) *e%TM#85iLfc4-yAyy ‘§IBK#i£^1BV'ry »y Kd b'yrx h£*#U y-f S’ o •7->yt1ftCf- xjbSrHIS t t t!cgj>jt!C|pll4fcff#SrtT9 ^£T*fo5>„ 7 ^y Kn b'yyy hTli, LT—«ttro«i-'¥lBBBB'y 4 ^ySrfflV'T, • #M&1f 9. -41- 1.1.4 [1] K. E. Petersen: Silicon as a mechanical material, Proc. of IEEE 70-5 (1982) 420-457. [2] S. Greek, F. Ericson, S. Johansson and J.-A. 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Ritchie: Cyclic fatigue-crack propagation in Magnesia- Partially-Stabilized Zirconia Ceramics, J. Am. Ceram. Soc., 73 (4) (1990) 893-903. 1. 2 9F%f£S • ftfrUrotfcSH 1. 2. 1 ■ iS;i (nilS§«) [l]:tll, xCffi, (£$§, 'J\JM : 9 3 Round Robin Test - 00-7, (2000), pp. 1-6. 1.2.2 (#3Mi L 1.2.3 L 1.2.4 L 46- 2. 2. 1 2. 1. 1 H&j yT<09F%M%*ffofc„ (1) aWt'-WilfSPS : Bl*l?t-ro;Sti«!IS*}o J; tmTf-ftM'lt 5Mmik»fa SrP^, 1*1 It X®3St£W&ft»&Sri#® Lfc. (2) 7 7 y R • □ t*y • 7-7. V (Round Robin Test) : gip|it!KM'®MM'fE)sSc*ft (s) ?i«K^w#igwsiift:*$e ®S*H-illt, j:5ftftftZ Off 9. K^»-*Bir'('Fricdnfc8«$7tl41#E/^-y^SSi:-rd„ Z®ft ft® S WftiifStt Srft W L (b)KftSSft : 7 y Xftitjb1 .tO'EeSEirfflV'Tt 7 7 yXftiCi bfc„ (4) gifK;BE®eS(b : *l$e$ftt© J: 9 ^IMimErojSA^TfiSrJlWL, SM"$«®* S(b^rff o7t„ Sfc. Ni 6MEff#Xc tx ^-7- K' : -74 7 n^-yyfi-iFK gIMM#, ##M#ft. Sift Abstract The aim of this study is the standardization of tensile test method of micro-materials. (1) Principle of micro tensile tests and measuring method have been studied in the previous works. The trend of international standardization has been surveyed. (2) The micro tensile test apparatus was newly developed as a microfactory cell and optimized for the Round Robin Test. Tensile tests were carried out on Ni-electroformed specimen and Si-specimen. The test results indicated the importance of the fixture method for specimen. (3) Micro grid pattern at 2 mm intervals is fabricated on a tensile specimen ’s surface by electron-beam- lithographic technique. The pattern is used to strain analysis in a magnified view of a optical micro scope or a scanning electron microscope. (4) Analyses of stress distribution and optimization of the dimensions of tensile specimens were carried out. Keywords: micromaterials, micro-Tensile Test, mechanical properties, standardization -47 2.1.2 -DV'TxE^<6 (1) (2) 7 Kn h 2) 7 Kn k'^T7 h (3) #:###]& 2) (4) 1) fftfrftj&y'&'i 2) (1 ) «UIMb^ 6. j: 9 LIGA7"n-1z7tC:%#yn±7;as:Er(7) «9 , 1^1#^ 6. (a) ###% (b) #t»—t ^4 9 n L<, mm, ^ ^ ny^-y- ^^b/t> 10(7)#^^#< , b/t# l(D#^(±m#:t> 10 // m(D^iJ^#V\ b/t 2^#50mm, R^(7)^@>15-e^)(9, y —1?#)# 48- d>&6o ( 2 ) 7 ^ > K ■ □ b: > • fX h (Round Rob i n Test) 1) umftimimomi, (c, bsu-8ic#LT7^ 6 (El2. i(A, B, 0), # )t^^(lEl2. 2(^^i-j:9^x ^TT^i|'M^s=100//m, Z(D#^ A ]; 7^7 7^—&(C 7 3- 7 7* K/vX h (Sl>8) IU2. 1 UV-LIGA ^$tr0.01 -49- ( 3 ) RRtiktttfiasafl: g| 2. 13 f (a)#fA#:(7)#0, (w j; z 6 of w K##f (c j; EI2. I9(^^f (2)&fR mwjmmt® Jfitfta mmmmt k (D sEivimmmm iz £ zm^-rn 1024x1024 2048x512 4096 x 256 8192x128 #% F= k- d2 A 0= d 1- 8 2 m2. 19 13 M" #2.1 ^Ittteif gwimmo) mwi&m® 025MHR 005MHR ±0.625 ±0.125 (mm) iSHtt 0.25 0.25 (±%) mm 540 306 (mV/ mm) — 58 — LV\ ^ C T, J^T(7) 3: 9 (a) 7 7 ^ (b) ^ 7 (a) 7 7 El 2. 23(C/^i-j: 9 (C, 9 Z 9 z^wi, "T##-c (1, n— 6 Z < f (9 , LT7 Lit. /b/c L, C <0£gffiCI«tl*Jt£ 7 "j'Pt^ El 2. 23 7 7^^it0tliSEl Ei2.24ic^i-z9ic, LT, <&rmv^, TZ^^Tf 7^y& fT9 (EI2.24). &»5 Z ^ ^:o Ei 2.24 Ei2.26(b)i:^ y j; 9 [C, ^ ^ n y(D^[#Wa#T$)6^, , ##(D% b #!#y 6 $) 60 2) urnxmwomMit m#:t, 6o j; 9 6Zn&mm^#m#fy7 h ANSYS l^TSFtFf L^ JEiS^ £r fr <5 fc0 $tK#^ol/''T{i, El 2. 27A ^ 2. 2 1^, ##^{#:(lEi2.28^^L^. 7^yKnk">T%b(cmv^il <57F^$c£rb t l^^ry1 V 'y y £rfro fz. ^y1 A^i'PMl^h'i, ^X tc CAD 'J 7 b Pro/Engineer Srffi $f, ^fT^*m^3oonm6L, OAW&fToTb, El2.29|C(j:, El 4:^(1, ^^^#^^gE#P^2#m^L^:. ±m^^fr^m^P=1.2P (#A^gE#P=P/ 1.2) ^^6(D#(D#^^Sg#P, Tm^^^#^P=1.5P (#A^eg#P=P/1.5) (D#(7)# 0 2. 27t*»*±^;i 0 2.28 A#. @$«S6fr ###{* y U ^ y 2. 2 ### \l";6 —K T^y# 160GPa 900 1200 600 zKTV^lt 0.33 1¥?I R3 R1.5+5 R10 300^m ¥nSMi y 5 umPrM S^im — 63~ 2 . 1 . 3 #gli (1) IT, t < irKM-d-SiroV'TlBSSrtTVX JIS/IS0#%6 t. (2) x ->y S • n e'y • yx h?rttuxo h x V T/vRM-ro^lSRSiSrmx 44 <£>*#* ft iroV'T^NSrfTofc. ifc, j: LTUV-liga . Ni##yot Xfr-oV'Tl&WLTc:, (3) : ^sntftt it, /tJM44S#fti: LTH. 7 x;7 Vit*5 J:t>'E*$:?-S:fflV'fcJ7 yy^ftiti: Lfc„ (4) : RSfcfrroVftj: LT, ¥fr95*B »-, «® t, ¥It95 *Sp, #AM EPBL, *952FSfl^fc5>„ * S1h£frxfc„ -Silt, #AMI@0L-2»', WasftS P=1.2L, M954M$R 2 5rdK 2. 1.4 #$%# 1) JIS Z 2201 ##:#4i (980/1990) 2) JIS Z 2241 AM##9l###*ft(1993) 3) JIS K 7127 y"y Xft y X X -f /PAS.U’y — h 03l36$tiltoft (1989/1994) 4) ISO 7500-1 Metallic Materials - Verification of Static Uniaxial Testing Machines - Part 1: Tensile Testing Machines First Edition 5) ISO 9513 Metallic Materials - Verification of Extensometers Used in Uniaxial Testing First Edition; (Corrected and Reprinted -1989) 6) /Nin#jc, w#, jwe# = ^#^^:#(F)(1993), 331. mm, B ^###^#73^^13^##^# (I) (1995), 360. 8 ) Staffan Greek, Fredric Ericson, Stefan Johansson and Jan-Ake Schweitz : In Situ Tensile Strength Measurement of Thick -Film and Thin-Film Micromachined Structures, Transducers’ 95, Vol. 2, p. 56-59. 9) M. Biebl and H. von Philipsborn : FRACTURE STRENGTH OF DOPED AND UND0PED P0LYSILIC0N, Transducers’ 95, Vol. 2, p. 72-75. 10) Shawn J. Cunningham, Wan Suwito and David T. Read : Tensile Testing of Epitaxial Silicon Films, Transducers^-95, Vol. 2, p. 96-99. 11) H. Ogawa, Y. Ishikawa and T. Kitahara : Measurements of stress-strain diagram of thin films by a developed tensile machine, Proc. SPIE’s 1996 Symp. Micromachining and Microfab- — 66 — rication, Microlithography and Metrology in Microraachinig II, Vol. 2880(1996), 272-279. 12) T. Yoshioka, M. Yamasaki, M. Shikida, and K. Sato : Tensile Testing of Thin-Film Materials on a Silicon Chip, 7th Int. Symposium on Micro Machine and Human Science, October 2-4, 1996, p. 111-117 13) D. T. R. and J. C. Marchall : Measurements of Fracture Strength and Young ’s modulus of Surface- micromachinig Polysilicon, Proc. SPIE’s 1996 Symp. Micromachining and Microfab rication, Microlithography and Metrology in Micromachinig II, Vol. 2880(1996), 56-63. 14) H. Ogawa, K. Suzuki, S. Kaneko, Y. Nakano, Y. Ishikawa and T. Kitahara : Measurements of Mechanical Properties of Mecrofabricated Thin Films, MEMS’ 97 p. 430-435 15) William N. Sharpe, Jr. , Bin Yuan, Ranji Vaidyanathan, and Richard L. Edwards : Measurements of Young ’s Modulus, Poisson Ratio and Tensile Strength of Polysilicon, MEMS’97 p. 424-429. 16) K. Sato, M. Shikida, T. Yoshida, T. Ando, T. Kawabata : Micro Tensile-Test of Silicon Film Having Different Crystallographic Orientations, Transducers’97, Vol. 1, p. 595-598 17) William N. Sharpe, Jr. , David A. LaVan, and Richard L. Edwards : Mechanical Properties of LIGA-Deposited Nickel for MEMS Transducers, TransducersJ-97, Vol. 1, p. 607-610 18) Wan Suwito, Martin L. Dunn, and Shawn J. Cunningham : Mechanical Behavior of Structures for Microelectromechanical Systems, Transducers’97, Vol. 1, p.611-614 19) David T. Read (National Institute of Standard and Technology : Piezo-actuated microtensile test apparatus, J. Testing and Evaluation Vol. 26, No. 3, 1998, p. 255-259 20) S. Greek, F. Fricson : Young ’s modulus, yield strength and fracture strength of microele ments determined by tensile testing, Mat. Res. Soc. Symp. Proc. Vol. 518, 1998, p. 51-56 21) G. Cornelia, R. P. Vinci, R Suryanarayananiyer R. H. Dauskardt, J. C. Bravman : Observation of low cycle fatigue of A1 thin films for MEMS applications, Mat. Res. Soc. Symp. Proc. Vol. 518, 1998, p. 81-86 22) W. N. Shapre, Jr. K. Turner, R. L. Edwards : Polysilicon tensile testing with electro static , Mat. Res. Soc. Symp. Proc. Vol. 518, 1998, p. 191-196 23) J. H. Tregilgas, M. Strumpell: Tensile testing of ultra-thin-film materials deposited on polyimide for mems applications, Mat. Res. Soc. Symp. Proc. Vol. 518, 1998, p. 179-184 24) J. Dual, E. Mazza, G. Schiltges, D. Schlums : Mechanical properties of microstructures : experiments and theory, SPIE Vol. 3225, 1997, p. 12-22 25) 1. Chasiotis, W. G. Knauss : Mechanical properties of thin polysilicon films by means of probe microscopy, SPIE Vol. 3512, 1998, p. 66-75 26) W. N. Sharpe, Jr. and A. McAleavey : Tensile properties of LIGA nickel, SPIE Vol. 3512, 1998, p. 130-137 27) S. Greek, S. Johansson •' Tensile testing of thin film microstructures, SPIE Vol. 3512, 1998, p. 344-350 28) T. Tuchiya, A. Inoue, andj. Sakata : Tensile Testing of Insulating Thin Films; Humidity Eff ecton Tensne Strength of Si02 Films, Transducers’ 99, VoLl, p. 488-491 -67 29) T.Yoshioka, T.Ando, M.Shikida, and K.Sato : Tensile Testing of Si02 and Si3N4 Films carried out on a Silicon Chip, Transducers’ 99, Vol. 1, P.496-499 30) T. Yi and C.J.Kim : Microscale Material Testing ; EtchantEffect on the the Tensile Strength, Transducers’ 99, Vol. 1, P.518-521 2. 2 m ■ ii;H - - mtwomR 2. 2. 1 ■ ii;n {uimm) p.235. [2] Y. Saotome, Y. Nakazawa, S.Kinuta : Microfactory cells for In-situ micromaterials and micro structures testing, Proc. 2nd Int. Workshop on Microfactories (2000), 982. 2.2.2 Lo 2.2.3 Lo 2.2.4 #k:%Lo — 68 — 3. 3. 1 3. 1. 1 Wftl ymxmxm&xtm%8r t hfvr *ta$ 5r-!7 - K : ^ D-7T y T/K 5I3W®, 5I3S3SS, 3WK Smt Micro-sized tensile specimens and fixtures fitted to the micro-material testing machine, which have been developed as a prototype in the Precision and Intelligence Laboratory, Tokyo Institute of Technology in collaboration with the Australia's Commonwealth Scientific and Industrial Research Organisation (CSIRO), have been designed and prepared. Tensile tests for micro-sized specimens were carried out using this testing machine. Specimens for tensile tests were prepared from a Ni-P amorphous alloy thin film and a 304 austenitic stainless steel thin foil. The geometry of the specimens were proportionally reduced from the ISO/JIS standards. Two types of fixture methods were used. One type was a micro adhesive method and the other was a hooked one. Similar mechanical properties (elastic modulus and tensile strength) were obtained for both the methods and these fixture methods are confirmed to be suitable for tensile tests for micro-sized specimens. Tensile tests were also carried out on trial specimens (SOI and poly silicon) towards round-robin tensile tests. The adhesive method was adopted for these trial specimens and tensile tests were able to carry out on the trial specimens successfully using this fixture method. It is therefore possible to carry out round robin tensile tests which will be performed in the next fiscal year. Key words: Micro-sized material, Tensile test, Tensile strength, Elastic modulus, Standardization -69- 3. 1. 2 PWStix k*-T h9!) 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T ----- g]3. • i 1 • i ! 1 i ----- 24 2 e : ; ; 1 ----- • 1 • i 1 • i ! 1 i ----- 4 Displacement • : 6 ; : : 1 ----- • 1 91 e _ i 1 e i 1 • r i 1 • i 1 / . * j ’ mm ■' 8 < > I e i — • i i i 10 i!i : ' : ; | i i i i 12 -- - i 41g©S»H D h 7-f r/m&ftmmy-^-y-y xah sttcimm l'*fUT+itolH XT-&V4h », @S£H::HilI/5v£Cfc„ 57tAlc, -ytosfcSAx Sifcj,£tW*;v^-roR|fa^ >g-efc5„ Jfm, yy-Aow^SS^J: 5K®^*AV-cfcd„ W^LW^. », §)A»fi*(ifWt«7c$|i^jfiV'^Witv\ ifc, e)A^7 y-A©M$T-SMLT WjVVc*, »to15WS-CI4*<, 2 3 4 fc, *0(0- yfffigBtl' jsij- 5. Skw&co-'O t^x. Biizdo s)RRTSs>rKtt, awjSAK^oTmM-K^y^tov'j:si-, tt5x^®y#nbivT t^5K Civ^m>tirJ:oTttff®Be^®»rLT*5 0, |iWb5Wiofdmc&oTV'5't) ro^#Bfcofc„ 4-#. r©^©Rff(-#*«s£-5i,i,^5o 4) W ? nS#i^V'd$*SJT*fc5d\ -yy =-yt^VT+^j:3M^*'t5S*SJ^ ,>'k<, mmsomm-k&mx'hZo **s, gtettii ltv '5$e#j*fl!v xhA 4-b® h7^r;vm 4-|c#LT«. +^*S*3SS^# feiv-cv '5^4 1M X^s $ 6> fck:# < &ofc i: S 1) K. Takashima, T. Kimura, M. Shimojo, Y. Higo, S. Sugiura, M. V. Swain: Proc. 7th Int. Fatigue Congr. (Fatigue 99), vol. 3, p. 1871, (1999) 2) Y. Higo, K. Takashima, M. Shimojo, S. Sugiura, M. V. Swain: Proc. MicroMat, p.997, (2000) 3) Y. Higo, K. Takashima, M. Shimojo, S. Sugiura, B. Pfister, M. V. Swain: Mat. Res. Soc. Symp. Proc. Vol 605, p. 241, (2000) 4) i*ftfD#, lE&AW, #SR-ffc, M.V. Swain: $T0fc, 40,184(2001) 5) S. Maekawa, K. Takashima, M. Shimojo, Y. Higo, B. Pfister, M. V. Swain: Jpn. J. AppL Phys., 39, p.7194, (1999) -92- 6) A. Ogura, Y. Ichkawa, M. Shimojo, K. Takashima, Y. Higo, M. V. Swain: Proc. MicroMat, p.574, (2000) 7) K. Takashima, S. Maekawa, Y Ichikawa, M. Shimojo, Y. Higo, S. Sugiura, M. V. Swain: Proc. MicroMat, p. 526, (2000) 8) K. Takashima, S. Maekawa, Y. Ichikawa, M. Shimojo, Y Higo, M. V. Swain: Proc. SEM, p.32, (2000) 9) Y. Ichikawa, S. Maeakawa, K. Takashima, M. Shimojo, Y. Higo, M. V. Swain: Mat. Res. Soc. Symp. Proc., Vol.605, p.273, (2000) 10) S. Maeakawa, K. Takashima, M. Shimojo, Y. Higo, M. V. Swain: Mat. Res. Soc. Symp. Proc., Vol.605, p.247, (2000) 11) K. Takashima, Y. Higo, S. Sugiura, M. Shimojo: Mat. Trans., 42, p.68, (2001) 3. 2 jtst. 3. 2. 1 ■ mm (aamm 3. 2. 2 XSt (###. * L 3. 2. 3 t£ L 3. 2. 4 * L -93 4 4.1 0F3EFjI#8<7>j££ 4.1.1 •7^ ^ □ -7'»R!m Round Robin Test ICteV'TIt^SS* Lfcl9$to|g$§r*tr4*BA#®^-y^'y rgi mmskxn t «#s«w%gif*s;, e b ^®#gi »w ®toi£ For the investigation of standardisation activities for the mechanical properties measurement of MEMS (Microelectromechanical Systems) materials, we have attended ASME IMECE 2000 and ASTM Symposium on Mechanical properties of structural films in the United States. For the investigation of recent progresses on the MEMS research, we attended the MEMS 2001 conference held in the Switzerland, and visited the ETH Zurich. In the round robin test, we have developed the fabrication process of the single crystal silicon specimens for the cross comparison trial that will be scheduled in the next year. We have developed the mask patterns of the specimens including the three types of the thin film tensile -94- testing method; that is on-chip tensile testing device of Nagoya Univ., the larger specimen for mechanical grips, and the smaller specimens for the electrostatic force grips. The mask designs are improved twice for a final design of the Round robin test devices. And the fabrication process for polysilicon specimens using the same mask designs as the SOI specimens are also developed. The tensile tester using the electrostatic force grip system is improved. A new chucking scheme for insulating thin films are proposed and tested. We also try to measure the elongation of the thin film specimen with the small marker on the specimen and the digital correlation methods are tested. Keywords: Electrostatic force grip, polysilicon, tensile test, tensile strength, Young ’s modulus, Round robin test 4.1 MMVfco Affctol-ii 2000¥ li M asmeIMECE2000, js r>* astm (American Society of Testing and Materials) (D Symposium on "Mechanical Properties of Structural Films"2001 ¥ 2 M 1^*4 MEMS2001 Ltc BW't&o ALT (2) Round Robin Test f^U RRT (l) 1) mm 7|eBT*HS5ilfc ASME (ry V IMECE2000, & £15 ASTM Symposium on mechanical properties of Structural films (C## U/c0 i£tc^ c? fife MEMS2001 Conference U ? n -ri/'sfrmoMcffiWftWjfa 6 t t 2) ^B^jottdlES ASTM (American Society for Testing and Materials) AM Ltz.D '*/ y^'yty ASTM L A. £/cx ASME(American Socitey of Mechanical Engineers) (DAS1I(IMECE2000)(£. t) titiJS Lx -95- MEMS L/Co »Bg 2000/11/6 : tti@ (Tieg Florida#! 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U—'sb y£p6f+S£ ^,T4ei9^ #%(Di/77A-e 10nm#^(D^##^#-e#5. ^#^C(D#&(D#mE §rfroTV>‘< ^^*Cfc5 0 4) $ £ #> 7 ^ ^ £: HB V fc0 ^N±yn-y±ic2c(Dmm, ^ 1 ocD@#$r#^L, 2 ocD^n —y±(DSS^^SESrOT VT, K# $^6@#(cz5#m^-e%#, 6ES&IWU Z^fp](D^i&^## 0.2 pm, 0.2 pm 4.1.3^# #6^^i±^T(D^4oK)'r^6o $ L-c, ASME (%y IMECE2000, 4oJ;U* ASTM Symposium on Mechanical properties of structural films (ZL# 134- tZ-o ♦ MEMS2001 Conference MSU W # P*rv'>'#Sf0|l£f %%§0#(D#%(co^Tmg L^:. ♦ Round Robin Test ^ y ^ i ^ ^ i ^ T y ^ ^ i mm##?) 1 —^^r##+L, Wir>y =* n -k % L^:o ♦ *?/ 6/N^L/c:0 Utzs c5 U'f^^#mT6#&$r^Lybo 4.1.4##3t# 1 Mechanical Properties of Structural Films, STP No 1413., C. Muhlstein and S. Brown, Eds., American Society for Testing and Materials, West Conshohocken, PA, in press. 2 K. Sato, M. Shikida, M. Yamasaki, and T. Yoshioka, “Micro tensile-test system fabricated on a single crystal silicon chip,” Proc. IEEE MEMS, pp. 360-365 (1996). : /J\HI, W:, A9-, fW, 1™5s,&V01.119-E N0.2 (1999), pp. 73-79. 4 T. Tsuchiya, O. Tabata, J. Sakata, and Y. Taga: “Specimen size effect on tensile strength of surface micro machined polycrystalline silicon thin films,” J. Microelectromechanical Systems, 7, 1, (1998) pp 106-113. 5 K. Sato, M. Shikida, M. Yamasaki, and T. Yoshioka, “Micro tensile-test system fabricated on a single crystal silicon chip,” Proc. IEEE MEMS, pp. 360-365 (1996). 6 C. Q. Davis and D. M. Freeman, “Statistics of subpixel registration algorithms based on spatiotemporal gradients or block matching, ” Optical Engineering 37(4), pp. 1290-98 (1998). -135- • !85t Stitt, 4.2.l@f%36S-I8;H (PUfBE) ISStJHI : Iptefl'yi) =iy©gi5I5S$fffi /Nnsx (x*s«K*«a«W9sff) %$56 : ? D-7i/ytyt-^f A|f9S£ (i# : 4.2.2XE (###&, 7k l 4.2.3#:f# 7k l 4.2.4i-0)#(D&# (^UX%EIF) 7k v -136 5. -tr-fn—rv/i,/ 5. 1. W3EHIKDJ** 5. 1. 1. ## LT, if«t ehttticEiv, Wy'n^-yy 5>mcjoV'T# 6 6(:®5S 20 y## m^mic^xLe^gtc-ov '?##&#% u^. -eroem, aT < /£5„ • 400‘CK-h-elS®a*43r^5 t, *B«##»%t:L, 4i6te#$ LfcT'n -try. £I8V 'T\ 35B1I' 3 U Round Robin Tfest Z'Mtia -rzt&K, ^^y*#d)*B#m, Ml:*lL, IsMOztettSrlfcET-#6S»m>trof^ ^f+lcoV'T S lb tcpitty — 9 lRS5r jo r * 5 „ r^f— v— Kj 9"^y#m, y y^\ tmah, *Bfi£, »a> afm In this fiscal year, we have investigated R&D trend about properties of thin films in the paper published in the 2000. As a result, there are many experiments for properties of silicon, but rarely for metal thin films. Furthermore, we have investigated research papers for -137- properties of titanium thin films for the past twenty years. As a result, we confirmed that there are hardly ever researches for property of titanium thin films. And, we planed the fabrication process for the three kinds of tensile testing specimens in one wafer for the purpose of the Round Robin Test. In addition to that, we implemented preliminary experiments and trial manufacturing of specimens. And, we have researched the grain size and distributions of atoms about titanium thin films concerning with thickness, process conditions and additional thermal oxidation. We obtained those results as below. • Titanium thin film surface becomes rough according to thickness of films. • Sputtering power has no influence on surface roughness of titanium thin film • Titanium thin films are oxidized in the air. • Progress of titanium thin film oxidizations in the air are deeper than aluminum and chromium thin films. • An annealing conditions does not have much effect on the percentage of oxide in the titanium thin film, but titanium thin films becomes thicker, the percentage of oxide increases. •Titanium thin film’s surface grain size and color transitions under the 400°C annealing. In the next year, we will fabricate three kinds of specimens and put into practice the Round Robin Test. And we will research the property of titanium thin films to make the standard sample of tensile test. [Keywords] Ti, Sputtering, TMAH, Surface roughness, Anneal, AES, AFM 5. 1. 2. (i) l) 9, WmMEMS lcS0-t5->5=.u-->3>y-A' tJEHLoofcti, $.tc MEMS tht'it LT, gFWICjb ’V'TSmSTOSft£jiTV —f a-r-yy-ftw-X'it, =■:/*, jyss, zKV •9, LTtl, B. CVD ') T/^5 -138 if)*, f ^ 2 ) 2000¥SjQSM9SiB$ 5.1 (^-r„ WS 139 - 5.i 2000 zwmotemR&i —iL tXBftjfMjjfe -yy^# Poly-Si te lmm 7 yyimm#Mi± 1) 5:5 12mm CVD 1#5 10~20pm 6 -yy^/# Si 5:5 100pm soim# 2) WrU'f^ te 40pm i¥5 5pm Si02 55 40pm FIB Surface profilemeter 3) # 25pm @5 0.6pm Poly-Si @5 0.9pm LPCVD+anneal 4) 4ty?3iA+ anneal -^y^# Si te 20~100pm soi mu 5) 55 6mm #5 3~5pm mmm PolySi 1#5 3.5pm LPCVD 6) Si02 IM 46pm TEOSCVD |o5 7) mmm 55 30~300pm "9## j?5 0.65pm -yyy# Si02 i|i@ l~5pm SOI (^#1L) 8) S13N4 55 105pm LPCVD m i¥5 2.3pm(Si0 2), 0.1pm(SiaN4) -yyy# SiNx - LPCVD mm 9) GaAs/InP @5 2—3pm MOVPE 10) wjsa NiSi J¥5 0.1pm SS+T ~—jV 11) -yyy# Ni J?5 4.4pm SSbSlT. h i//f y-fey-tt 12) 3lo3g9%# 55pm ms Ty^ Si te 200~800nm AFM (cj:5^# AFM stfm 13) (Nano-wire) 55 6mm i?5 255nm (2) Round Robin Thst Jfjiptilfcji k 1) ## jsv 6^,TV ^6##5I 0 $##c Z 6o Z(Dfzhb\at^\^'O^BKMLX Round Robin Test ^a5i-Dgg 19 ##-e#6z 9 ^yntL. o^< c ^^ #$ LVV 140- *W%Trtt, V >^'ailcJ:oT/i8i8Lfc9 u^y»R5r5lo«y LTiWlLfc, i 2) yy 3ym*emv'T?- lA'L TMAH ^mitmr/uij yWtfcx&ztztb, -fKii&RSigto#* 6jTd„ ^ntztbx- 7 y##(7)M#^M#ICj3V 'T TMAH TMAH yWRlcXtS -Rg^KoV'T^Ni"d£-S»sfc-5. 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AI V k'-zf ] : 'y 1J ^ y I I : T/^zzr^ mm : 5. mm El 5.7 Round Robin Test "7° n i? y -148 - 5) dr* , Round Robin Test Xf fzCj 5.8 fRl— V^/^±LjoV'T 3 fo LI LI El 5.8 Round Robin Test 5.2 s L m 19 z rmm mix* te [pm] iE $ [pm] « M 50 100 10 20 100 3 50 100 2 20 100 6 ««s«w9zm 50 500 1 20 500 1 300 500 4 50 100 12 20 100 12 50 500 12 20 500 12 -149 6) Lfcr/nTyTIfjl't, Round Robin Test fflKftflifMZte ;4'o fc, y-y#tit£y y -x-i- sb#,6ts m^BSis*hi o rm jreM%# tr t* t\ #@$y '11'5 c-cva, iWJtHjoV 'Til, Round Robin Tfest y#E 7) £ 1) 18$ IfjliiT'it^c^^y^loKyKK^TiffKTn-fey^fflV'dr jilCloT, in—<7)'7z/n ±IC 3estoS/idswr&fiSH-d : 2) fi0E*&ro«@ L/txTiy? y yT#l=169"^y#mi, (J yitifi lt, L/cfcd -150- 5.3 EJ¥tc*l-t-5¥tS*B6£ j]W VSBfiS (R») ¥J6BES/jgiV 2750 A 8.1 nm 2.94 % 5000 A 12.4 nm 2.49 % 7900 A 15.1 nm 1.91 % 19000 A 26.4 nm 1.39 % 29000 A 29.8 nm 1.04 % 39000 A 37.8 nm 0.96 % 51000A 53.3 nm 1.04 % WW<7k5l$if*Be5^*S: < £V'5 C£;m®T*Sfc;S\ VSBE $A51. < &oTV ' 6. (-Lfcfc®^, 0 5.12 T?*>5„ rro«[p]lc«5 i:, x /n >? y y^'8felcJ:-6#reKMLrttfle»^W< *Be£roi?8lt/h£< *otV' 4-811. *bic#k § i o ® y i-wr srfm l. V'TltW4ril»rV'<„ 3.5 3 2.5 Bt B 2 \ •W 58 1.5 @ g 1 I* 0.5 0 10000 20000 30000 40000 50000 60000 BIS [A] 0 5.12 ro:(r^-f5¥^@E5(DWJ^ 4) ^>mm -153- w % 2* 4 w #d RELATIVE CONCENTRATION (X) S £ (4 hr d ft ft a z 5g& Hi o'"' § § M 4 M" $ 3* ft 4 O'* rv & #94 Si (4 m m FF lit- m w r rv a r ft % null 0 d ° f (4 3h Si ft 2000A 2 0 200C 5 in 15m i—> On LO 0 3 t l i t 3 -f ofc^g-rofeS&EI RELATIVE CONCENTRATION (%) &.± File 3 ■y-yy : 03121BZ.SDP ’ si'&im-fZ) 5.25 0 5.25 /j>y%l Ti SPUTTERING SOOOA^f 5000A t 5.27 , (EWtS&U non ( '-T^"t, 40 TIME Heat - 2oooA(c#6 162 2000 (Min) tilt30 - A mmc, 'taz-6o mites S*iB] . V V . T 0.1 0.9B*10~ Line 179.32 80.00 85 95.0 10.00 10.00 *10 3.00 6 Gain k mV kV eVp-p A min min kV /min * RELATIVE CONCENTRATION (X) RELATIVE CONCENTRATION (X) T1 i T 5000A 5000A O H N2 2 0 200C 200C 5 In 15m 5 in 15m CTi CO 0 3 t l i t 0 3 t l i t 3 D £-f0 5.25 ICjolt5SW!fa*L(7)»S-(D|S$Srft5 3>roM$tr#6L'rv'5„ ctu-t'pt£< t h soooA^m&ix^ 9 ycomit^mn l-o '3 z t ^ L-a '5. Stic, KJW 5000Aco#6ll, ## 2000A 5000AMR|c*hf5 400‘Crofl®a B^aBE^f y##lc*r6B#&MW'lcr6/bAlc, 400:Clc±sfT, SSSHS* £ K*#H«4’ie*3H 6B4aa®i5Steov 'T#I4*4= : *o A. MstMliR C < 15 5* £ U ^ySIgiTffSt 5000A£ LT1'5„ AFM ofct<7)^yTie^-f-„ 0 5.28 soooAro^^40or, i5»MB»a £jb'£7fco/ctc7), 0 5.29 HR C< 5000A <0 -£ S’ >iWA @S#05VI ’ A 400C, 15 ®a&&£&ofet —164 6) A 9 y##& DC 7" U—-)~7 h a yx/< y 9 V y 9 ’igtlz =t o TfiKR L, ?-7 iass*iS]©msfticov'T, e-*e#&emv^?>mmimi'X&.T(D£ ?%%>&$; #6 *1\ filiittrtltlKiLtli, =f7y$IS|j:K»W< *9, v -/?'mtz£'}Tfmi.tc7L9>&m iTt, 9 L^y#Ett*S4,tr@ceLr*5< t, 5000A 6$OS»*6,(izE5*|6lS:f*:irj= ‘V'TWtoiiefrtS r i: lC@Hb»Sii*lH,1~V*® -167- 5. i. 3 isn lt, 20tK)¥®c43V'TBrtfl--e«*£ iLztWE®St6to#l4irMt"-5to3z:i;ov 'T, -Erto^tstfS^S^*&lc-^>v 'TUSSr 43A ft o yt„ SAIA Round Robin Test mmkKtmoMcmklCfartX. Round Robin 1fest-efflV'd3a#(Dg|oMl9m>t(D#iSjb- rjxBcoRKjtSrll] —5,z/N±tcs5^(covL?t. riL^rolS$x KTCiJ: • 2000 3ctt?s#ic*3V'T'>y 3 y MtiSR- /tt 5 SlSUjy 1Atiir • T/V5 = r>^^«eifc‘J:^x5ry^)l^ LTfflvx TMAH, V') =iy, jg«ry^= 9 -y9^y^i^ib LTT^V-'6C^(Cj:c-C, 9* A y^DBIAffltyfc Round Robin Test mmtmnmi-z ~ t tfsimx-hz* • V y^'&Kj:c-aiKmL^9f y#m«R*aw< *Bfi£as*§< & <5o • g&##icj3i46^/ 5. 1. 4 ##3t®t 1) #0% m##fii, fiiSJHK, " -79 ^ □ -r->yfl 7 yytcESSE CVD (Ofi0B#t@F% -;Ky -yy ayl©ig6<)fitti < Lit-T-AroltfTA Vol.66, No.9, 2000, p 1421-1425 2) SIWA-y?, tes-tt, " #m##A**&S6^y9yygl***K i-y^fAOir , Vol.66, No.12, 2000, p.1890-1894 3) S.Reyntjens and R.Puers, “Focused ion beam induced deposition: fabrication of three-dimensional microstructures and young ’s modulus of the deposited material”, Journal of Micromechanics and Microengineering 10 (2000), p. 181-188 -168 4) H.Bemey, M.Hill, AK.Kelleher, E.Hynes, M.O’Neil, WA.Lane, “Investigation of the effect of processing steps on stress in a polysilicon structural membrane”, Journal of Micromechanics and Microengineering, 10 (2000), p.223‘234 5) Taechung.Yi, Lu.Li, OJ.Kim, ‘Microscale material testing of single crystalline silicon! process effects on surface morphology and tensile strength ”, Sensors and Actuators(A), Vol.83(l-3), 22 May 2000, p. 172-178 6) H.Kahn, N.Tayebi, R.Ballarini, R.LMullen and A.H.Heuer, “Fracture toughness of polysilicon MEMS device”, Sensors and Actuators (A), Vol.82A(V3), 15 May 2000, p.274-280 7) Toshiyuki Tsuchiya, Atsuko Inoue, Jiro Sakata, “Tensile testing of insulating thin film ! humidity effect on tensile strength of SiC>2 films”, Sensors and Actuators (A), Vol.82A(T3), 15 May 2000, p.286-296 8) Tetsuo Yoshida, Taeko Ando, Mitsuhiro Shikita, Kazuo Sato, “Tensil testing of Si02 and Si3N4 films carried out on a sihcon chip”, Sensors and Actuators (A), Vol.82A(l"3), 15 May 2000, p.291-296 9) R.Kazinczi, J.RMollinger, A.Bossche, “Versatile tool for characterizing long-term stability and reliability of micromechanical structures”, Sensors and Actuators (A), Vol.85A(T3), 25 August 2000, p.84 89 10) E.Peiner, K.Fricke, I .Behrens, A.Bakin, ASchlachetzki, “Hetero-micromachining of epitaxial III/V compound semiconductors ”, Sensors and Actuators (A), Vol.85A(T3), 25 August 2000, p.324*329 11) M.Qin, M.C.Poon, C.Y.Yuen, “A study of nickel silicide film as a mechanical material”, Sensors and Actuators (A), Vol.87A(l-2), 1 December 2000, p.90*95 12) L.L.Chu, L.Que, Y.B.Gianchandani, “Temperature coefficients of material properties for electrodeposited MEMS”, Proceeding of MEMS2001, p.68-71 13) Y.Isono, T.Namazu, T.Tanaka, “AFM bending testing of nanometric single crystal wire at intermediate temperatures for MEMS”, Proceeding of MEMS2001, p. 135-138 14) 3emH\ t X>iT^(DB\Jg\ E 0, 119 #2#-, 1999, p.67;72 15) /Jnjuwx wmm-. HElcDSJS”, mm## E0, 119#2^-, 1999, p.73-79 16) ±m#A, m^#^E#,199# 5 1999, p.290-294 17) Gui zhen Van, Phihp C.H.Chan, I Ming Hsing, Rajnish K.Sharma, Johnny K.O.Sin, “An improved TMAH Sketching solution without attacking exposed Aluminum”, Proceeding of MEMS2000, p.562-567 -169 5. 2 m%§m • am* xm. tssutoKiH 5. 2. 1 ■ mm * L 5. 2. 2 X® 7k L 5. 2. 3 ##f# #ff : (mm##2001-01743?) 5. 2. 4 -eotero^s Cfuxa##) 7k L -170 6. 6.1 6.1.1 m & Round Robin Test (RRT) (C^V C ^ B yy ^ ySSt ( 100mm ^ M £ 525 n m) 6 ^ y ^ ^#2^m±0.2pm^Bmc^'g icov\T##L^o o.5iA/dm\m#m 26.7min =z>&#(D(f)70mm (D^g^lCjoV^Tg##^# tcov^##L^o %#, mrn^^o.5iA/cm2 80-120MPa^^5o 100-400%:)^9 ^ 163-782MP& J¥£ 2nm(D~ '7^o^I© RRT f*Wf£ Abstract In order to stabilize mechanical properties of thin-film specimens being used for Round Robin Test (RRT), we made studies on evenness of Ni film thickness and stability of residual stress of Ni plating film on Si substrate (100mm-diameter and 525pm-thickness). We decided on a target of 2 ± 0.2 pm of Ni film thickness and made examinations on plating conditions to determine the optimum current density and deposition time. As a result, we adopted 0.51 A/dm2 as the current density and 26.7 minutes as the plating time. We confirmed that the evenness of the thickness is guaranteed when we adopt these plating conditions and fabricate specimens from the 70 mm-diameter portion of a 100 mm-diameter wafer. We also determined the effect of plating conditions and heat treatment on the residual stress of Ni plating film. We used X-ray diffraction to measure the residual stress. When the current density is higher than 0.51 A/dm2’ the residual stress is between 80 and 120MPa and changes little. As for heat treatment, residual stress increases with the annealing temperature (KXM00°C). Based on the results above, we have fabricated some RRT specimens of Ni plating film with 2 pm thickness on a 70-mm-diameter portion of a 100-mm-diameter Si wafer without annealing. Key words; Silicone substrate, Thin film, Plating, Residual stress, X-ray diffraction, Deflection, Deposition condition -171- 6.1.2 (1) Round Robin Tbst (01$uM -74 4 Round Robin Tfest (M$, RRT 416®) rid:, W&Wfecti^o#z)S'>4v5 4 t ^8$rfcd„ i»JR -172- (2)zbO^%W'%Z9(c, ##±"% IF =96,490C(=A- s)(D@#^Za, Ni (D#m#^M/2T^aC(bZ9, #^"f6 Ni (DM W2#(4)ztT#i-Z ^ 60 M I -t W, (4) 2 96,490 Ni w^ =w, ^^ao-e, . M I -t p • d 2 96,490 M I d (5) 2 x 96,490 xpS .-c, i/s#mm#Eo-c&ao (5)^i(6)^:(DZ9(c^$^,ac d =------G • t ...... (6) 2 x 96,490 x/? rrt% (6)^- Ni (Djj^Fi;M=58.7, $£Ep=8.9 (20%:) 3)§rftA-f&b. (7)^0 J: 5 Ni (D^Epd, (50-60T) T#, dcal—0.205 x cr x t ...... (7) ^(D^-o#KjdV^-CflNi(D#m^#(:#^$)9, (7Wc^Lt#t#5% dex= 7j x 0.205 xcrxt ...... (8) c(Dj5%^Ms„%\ 2(D^(cov^-c^#T^ao 6.1 \z^t0 iim & (100) (EH 100mm, E@ 0.525mm, n^, #%#0.1-1000 cm) ~?2bZ> 0 '>]) )6o#(DT%## £ LT7"^y CTD (##50nm) RXM l (An) Xs