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1 Journal of the Ceramic Society of Japan 115 [3] (2007) Paper ê ñ é ü ~p ó t píêéåöíüéåáåö çñ j~åüáå~ääé dä~ëëjáå~ `çãéçëáíéë Osami ABE and Kazuya KOURIN The Research Center for Superplasticity, Faculty of Engineering, Ibaraki Univeristy, , Nakanarisawa-cho, Hitachi-shi, Ibaraki The effect of additives has been studied to improve the strength of machinable glass-mica ceramics. Titania, Y 2 O 3 -doped partially stabilized zirconia Y PSZ and celsian Ba 1 x Sr x Al 2 Si 2 O 8, x 0, 0.1 and 0.2 powders 10 mass were mixed to the previously prepared glass-mica powder content of F-flogopite: 45 vol by using a ball mill. The ball-mill grinding without additives improves the strength from 144 to 172 MPa through the size reduction of mica grains and the increase in sintered density. The addition of TiO 2 and Y PSZ is more effective to the microstructural refinement and the strengthening 190 MPaTiO 2,220MPaY PSZ. Y PSZ particles are segregated to the longitudinal ends of mica grains and suppress their longitudinal growth. It is expected that the Y PSZ particles act as the reinforcements to the glass matrix to enhance the strength. The growth of titania particles under sintering results in the limited effect to structural refinement and the smaller strength than that for Y PSZ-doped materials. The addition of celsians is further effective to the size reduction of mica grains and related densification to improve the strength MPa markedly. The celsian particles do not show their coarsening as well as Y PSZ, and dissolve to the glass phase during sintering gradually. It is considered that the dissolution of celsians suppresses the growth of mica grains by changing the chemical composition of the glass phase. The increase of Young's modulus of the celsian-doped glass phase should also contribute to the strengthening. Received September 15, 2006; Accepted January 18, 2007 Key-words : Machninable composite, Mica, Strength, Microstructure, Grain size, Titania, Y PSZ, Celsian ü ó íñ Ù ˆ ó íñ 1 ê ñ š Ý é ü ó íñ 2,3 ê ñ é ñúü ú ï ý ù ý n ~p 1,4 é ÙÛ ü Ý ê ñ é ~p Ý 100 MPa Û Ò é Ý Ò Û 5,6 ü ð ú 7 Ú Ú ~p ò pý ò Ò 1500?C ý 2 Ý ý Ý1300?C ê ñ nõ é { v 8 Ú Ò ê ñ é Ý r Ý ù ý ú ð ý Y PSZ Ê 3 ó Ba 1 x Sr x Al 2 Si 2 O 8, x 0, 0.1, 0.2 Ý ù ý Y PSZ é Ý ý î Ý Ý Y PSZ Ý ê ñ ú íñý n Ó ó º Ó ê ñó íñ Ó 9 11 é ý î Ý Úê ñ z 2 Ú ~pý r p p ê ñ é 45 vol šý K ï ú ó ú SP p šù SSA 10.0 m 2 g 1 Ý 12 p TEM Ý é é ê ñ Ú 2 3 mm é Ó ÒÚ ù ý Fig. 1. Morphology of staring glass-mica powder. 216

2 Journal of the Ceramic Society of Japan 115 [ 3 ] Ti i OPr 4 Ý œ Ý600?C 2h º Å ü ô ù Ý ð ý Y PSZ HZ Y3M 3 mol Y 2 O 3 Ó600?C 2h º Å 3 ó Ba 1 x Sr x Al 2 Si 2 O 8, x 0, 0.1, 0.2 B100, B90S, B80S h 10g Ù é SSA 300 m 2 g 1 g ü SSA 158 m 2 g 1 Ê Ba OH 2 8H 2 O Sr OH 2 8H 2 O Ó ë ë Ý v ï Ê ÙÛ óú 3 s 1 2h œ 1000?C 2h º Å 13 Ð r 9 ë ó Ú Ý v ÙÛ óú 2.5 s 1 1h a» ó p œ œ Ý Ò º Å êñ œ î íñ ø SSA 18.1 m 2 g 1 ù ý 14.2 m 2 g 1 Y PSZ,11.8m 2 g 1 B100,14.2m 2 g 1 B90S, 12.9 m 2 g 1 B80S ù ý Ý Y PSZ Ò ê ñ é 18 g 2gÝ ï q10 mm Á 0.30 Ê 80 cm 3 Ó 500 cm 3 ÙÛ n 2s 1 15 h» 85?C Ì 60 š Ò Ý Å Ýø SSA 16.3 m 2 g 1 Ó Å p Ý M Å Ýr Ý G ù ý Y PSZ, B100, B90S, B80S Ý Ý T, Z, B, N, E Ú Ýð ý Û Ý mm 17 MPa z 150 MPa œ CIP F Ý ú Å TMA Ý œ º 5K min ?C 1 min r 1100?C 2h ~p q Ý 4 3 mm 1 mm ø û ñú Û ?C r Á2000 SEM Ý 2 þ mm 4 þ œ š Ú Ý Ò 0.05 mm ë ñ r bulk Ý r bulk r Ú Ò r R Ý œ Á P C 1250?C r P C ë ñ Ò r R Ý M G 1100?C r R g cm g cm 1 X Å RAD C Cu Ka 40 kv 20 ma s f ñ 10 mm í ñ ûñ û0.5 mm min 1 3 y ñú 2282 é ñ H V Ý0.1 mm é ñ ð Ý 98N u HV114 K IC Indentation Fracture Evans Ò Fig. 2. Influence of ball-mill grinding G and the addition of titania T and Y PSZ Z on temperature dependence of shrinkage rate F. M: as-supplied. Fig. 3. Microstructure of sintered materials M as-supplied and G ball-mill ground at 1100?C 2 h and 1250?C 1 min. Ý0.1 æ ù î SEM ÿ t S 4300 SEM Ú 200 é d eq d L d T ñ íúš A Ý îá E ñ t ü ú íñ 5800 Ê M G T Z F Ý Å M 1000?C ø 1100?C íý 2 ø í 1100?C 2 h 1250?C 1 min Ýÿ Ù Ú Ó é ê ñ ú íñ n Ý é í œ r Ê œ Á P C Ýù Í j d L C 1.31 mm Ì1250 C 2.88 mm Í Ì1100 C 3Ý4 j

3 218 ê ñ é ü ~p Table 1. Density and Microstructural Feature of Sintered Materials 1 mm Ì1250 C j 5 mm Í 1100 C j Ì Ì1100 C j Î Í Ý p Ý Å šù 10.0 Ú16.3 m 2 g 1 2 F Ó1050?C Ž r 1100?C 1 Ú 1050?C F ù 1 Ù 1250?C M ÙÛ Ó é d L ?C 1.21 mm 1250?C Ó2.32 mm M ÙÛÓ 3 SEM Ù 1100?C n œ ÿ œ u Ó œ Ó œ n Ó Ê Ú Ý Ò é Ý ?C œ Ý ý ù ý Ê Y PSZ 1100?C 2h ~p X Ý M G p š 3T 1M Ý T Z ü ô Ú ù ù ý r Ý Y PSZ 2 y T Z F ?C G šð Ý ù 1 Ó1100?C ?C T Z Á SEM Ý M G š ~p Ó0.5 2 mm é ÒÚ T ù ý šù Å 0.08 mm ÒÚ ù ý é Ê Ú 5 Y PSZ šù Å 0.07 mm é ÿ é d eq 0.25 mm n Ý T ù ý Ó Å M Å G šð T G uú ù 1 Ù ñ íúš A av Ó Ú Ù é Fig. 4. X-ray diffraction patterns of sintered materials M as-supplied, G ball-mill ground, T titania addition and Z Y PSZ addition. Sintering: 1100?C 2 h, F-Phlogopite 1M, F- Phlogopite 3T, Y PSZ tetragonal, Y PSZ monoclinic, TiO 2 rutile. Fig. 5. Microstructure of sintered materials T and Z compared with M and G. Sintering: 1100?C 2 h. Allows indicate Y PSZ particles at the longitudinal ends of mica grains. r uú Þ Y PSZ Ý 1100?C Ê Ú Õ ù ý 2 Ó ?C F Z šð T Z y 1200?C Ê ÒÚ 1250?C 1100?CÙÛÓ Ú þ œ Ó Ý ê ñ Ê Ú ó 3 ó Ý B N E y Ý ó Ý Ý 2 T Ê Z š

4 Journal of the Ceramic Society of Japan 115 [ 3 ] Fig. 6. Distribution of equivalent size of mica grains d eq in sintered materials M, T, G and Z. Fig. 8. X-ray diffraction patterns of sintered materials B, N and E. Sintering: 1100?C 2 h, F-Phlogopite 1M, F-Phlogopite 3T, Ba, Sr Al 2 Si 2 O 8 monoclinic. Fig. 7. Influence of the addition of BaAl 2 Si 2 O 8 B, Ba 0.9 Sr 0.1 Al 2 Si 2 O 8 N and Ba 0.8 Sr 0.2 Al 2 Si 2 O 8 E on temperature dependence of shrinkage rate F. M: as-supplied. Ó ó ?C F ñú ù h ó Ú 7 y 1120?C œ Ó Þ Ê Ú 1250?C ù 1 Ù 1100?C X Ý š 3T 1M ÒÚ ó í ÒÚ š 1M 003 3T 009 í M Ú SEM Ó 1100?C ó Þ ÿ 1080?C 2 h Þ ó ê ñ ó é Ý T Õ Z šð F 1000?C ê ñ Ú Ý 1100?C Ê Ú 1100?C Fig. 9. Microstructure of sintered materials B, N and E. Sintering: 1100?C 2 h. Allows indicate celsian particles. B é {Á SEM Ú43 Ò Ú M 45 šð Ù ó ÝÊ Ò 1100?C ó é d eq n Ý Ýù 1 ó d eq Ý 6 š B N E mm T Õ Z š Ó 0.5 mm ù 1 Ú ó Û é ð d L 50 Ó ñ íúš T Õ Z M Õ G Û Ú z d eq ñú ù Ù h Þ Ú 7 y ó

5 220 ê ñ é ü ~p Table 2. Mechanical Properties of Sintered Materials Fig. 10. Distribution of equivalent size of mica grains d eq in sintered materials B, N and E. ê ñ Ù Ó Ê Ú é T Õ Z Ù Ù uú Ù ó Ù ê ñ é þ Ý Ó Ê Ú 1250?C ÒÚ ó ê ñ Ó è 2 s Ý ê ñ œ Ó Ó e è šð è ñú ù è ê ñ Ó Ê ù ?C B N E ˆ 1100?C ~p ˆ Ýù s f é 90 d L 90 rƒ n Ý Ú Ð 4 5 Ò Å~ M JIS R 1601 ñ 30 mm 3 y 121 MPa šð s f d L Û Ý uú B Å Û Ú r Ú Ý n Y mm M 14 mm E Û Ý n Y Û Ó15 mm M 5 mm E d L 90 ÙÛuÚ é í œ Ê Ú é Ý œ Ó Û Ê Ú G Å Ù 1 Ù s f 177 MPa T Z Ó97 Ó Ú Ù s f 190 Ê220 MPa d L 90 d L 50 Z H V K IC Fig. 11. Dependence of fracture strength on reciprocal root of longitudinal size of mica grains. Ú Y PSZ Ù ê ñ ú íñ n e Y PSZ Ú Û Ú ó zó H V E Ó ê ñ Ù îá Ó Ê Ú Ó Ý ûû Ù 3mm 1mm Ê 3mm Baik Ú 15 ê ñ é ~p ü H V K IC 2 Ýg Û 10 mm 1 Ti C, N ú Ý Û 0.5 mm 1m min 1 ~p Ð Ý Ý Ê Ú ê ñ é ü ó íñ Ý Ý Ò ù ý ú ð ý Y PSZ Ê 3 ó Ý šý45 vol K ï ê ñ pý

6 Journal of the Ceramic Society of Japan 115 [ 3 ] Ó é Ý Ú Ó 2 Ú Y PSZ Þ é Ý Ý 1.5 Y PSZ Ù ê ñ n Ó ó Å~ ó Ó 1000?C ê ñ Ú Ê Ú ó Ý ê ñ î Á Ó ø Û p Ý g ì SEM ÿ øó ì References 1 The Ceramic Society of Japan Ed., Handbook of Ceramics 2nd ed., Application, Gihodo-Shuppan, Tokyo 2002 pp in Japanese. 2 Grossmann, D. G., J. Am. Ceram. Soc., Vol. 55, pp Grossmann, D. G., Am. Machinist, Vol. 122, pp Kusunose, T., Sekino, T., Choa, Y. and Niihara, K., J. Am. Ceram. Soc., Vol. 85, pp Uno, T., Kasuga, T. and Nakayama, S., J. Ceram. Soc. Japan, Vol. 100, pp in Japanese. 6 Uno, T., Kasuga, T. and Niihara, K., J. Am. Ceram. Soc., Vol. 74, pp Uno, T., Kasuga, T., Nakayama, S. and Ikushima, A. J., J. Am. Ceram. Soc., Vol. 76, pp Miyake, T., New Ceramics, No. 5, pp in Japanese. 9 Lee, W. E., Chen, M. and James, P. F., J. Am. Ceram. Soc., Vol. 78, pp Liu, C., Komarneni, S. and Roy, R., J. Am. Ceram. Soc., Vol. 78, pp Chinn, R. E., Haun, M. J., Kim, C. Y. and Price, D. B., J. Am. Ceram. Soc., Vol. 83, pp Kourin, K., Takata, S. and Abe, O., Proc. of Ann. Meet. on the Ceram. Soc. Japan 2003 p. 96 in Japanese. 13 Ohkuma, H. and Abe, O., Proc. of Fall Symp. on the Ceram. Soc. Japan 1995 p. 431 in Japanese. 14 The Ceramics Society of Japan Ed., Evaluation of Mechanical Properties of Ceramics, Gihodo, Tokyo 1979 pp in Japanese. 15 Baik, D., No, K., Chun, S. and Yoon, Y., J. Am. Ceram. Soc., Vol. 78, pp

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