Synthesis and Characterization of Titania-Partially-StabilizedZirconia by Ultrasonic Spray Pyrolysis TPSZ

전체 글

(1)Journal of the Korean Chemical Society 2000, Vol. 44, No. 6 Printed in the Republic of Korea. TPSZ

(2) *. (2000. 8. 5 ) Synthesis and Characterization of Titania-Partially-Stabilized Zirconia by Ultrasonic Spray Pyrolysis Ki-Lyong Seo and Chang-Seop Ri* Department of chemistry, Keimyung University, Daegu 704-701, Korea (Received August 5, 2000). .

(3) , TPSZ(titania partially-stabilized zirconia) !"# $%&'()* +

(4) +,-., /01 2 !34 56 # 78+9, : 2# ;+,<. =>?@ A4 BCD 0.025E0.1 M F G HI ?)+9, J K4 ZrO 90E97.5 wt% TiO 2.5E10 wt% FG +,<. L ( ) 5M 4 NO 400E550 C, PQO4 800E1100 CR +,-., : 4 ST-R UV+

(5) 110 C 3LW XY N+,<. : ! 2# Raman Spectroscopy, X-ray diffraction(XRD), Scanning Electron Microscopy(SEM), Transmission Electron Microscopy (TEM) Particle Size Analyzer(PSA)RZ ;+,9, Inductively Coupled Plasma-Atomic Emission Spectroscopy(ICPAES)RZ [ # \+,<. 2. 2. o. o. o. ABSTRACT. The fine particles of binary ceramic composite of titania-partially-stabilized zirconia(TPSZ) were synthesized by ultrasonic spray pyrolysis at the various temperatures, compositions and concentrations and the effects of process factors for synthesis on the characteristics of fine particles were discussed. The starting salt solutions were prepared to have the ionic concentrations of 0.025~0.1 M aqueous solutions. The fine particles were prepared to have the compositions of 90~97.5 wt% of ZrO2 and 2.5~10 wt% of TiO2. The temperatures for particle synthesis were regulated to be 400~550 oC as a drying zone, 800~1100 oC as a pyrolysis zone. The produced fine particles were collected by a wet process and analyzed to investigate characteristic properties after being dried. The compositions of ceramic fine particles were determined by Inductively Coupled Plasma-Atomic Emission Spectroscopy(ICP-AES) technique and phases, morphologies and particle sizes of those were investigated by Raman Spectroscopy, X-ray diffraction(XRD), Scanning Electron Microscopy(SEM), Transmission Electron Microscopy(TEM) and Particle Size Analyzer(PSA) techniques.. ]^ _ à, b Vbc d è fg:<. d Aah^ &1 i jk lg mn+., J A o*^ 9 pq (), ab @b-ROr \= sPt<. 1. 9 p4 !u A+4 v sPt1 o *w, ax aj y zD, p_{|} QV y y ~ Aq pa I pN d _ àq b, U ! y ~ è <. 9 ()4 BC 'aDx aD# ()+4 o*-R 592.

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(14) a Õ <Ö I « # × +Ä Á(Ø »( ÙÚ+e ¬Æ. u Y0 ÈÉÊÆ(partially stabilized zirconia, PSZ) y<. 91, 9Ø 3Ûy Õ¢u A+a ±) Ük" nÂF4 ]^ sPt-R ! 9 Â., _ U Ý9 9[., QV + Þ9 Y0 AR ;?F4 ! Ás+e 2. submicron. 3. 4. 5-8. 9-14. 593. UFß y<. y 2# wàLá4 "# +a ±+

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(16) Ü¾ _ b# +a ãë ¡ ¿ <. J x $%&'()*(ultrasonic spray pyrolysis, USP)^ ìí BCD# ;?+

(17) ?@-R w{9, { ?@# $%& 'aR !+e ' +

(18) , aR î^ LW ()Lá½R Ás+9 ¢0]., _U Ý9 Â ! Ä QV+ Þ4 9[ bt1 Ük "# # 4 lg ¬^ o*<. d ï Â4 BC é;æ ?@# $% &'()L ðçÊÆ Y0 ÈÉÊÆ(TPSZ) !u A+,-., ?@ , ()L PQLW ~ dÖ 2#

(19) \o*-R ;+9, $! AL tN# Â+,<. 18-24. . ï ñò ;?: $%& '()v3 óôu Fig. 1 xç»<. ñòv. 15. 16-17. 2000, Vol. 44, No. 6. Fig. 1. Schematic diagram of ultrasonic spray pyrolysis system..

(20) . 594. 34 $%& @t >v3, NO, PQO, U Vv3 4ó O-R ÂF<. $%& @t >v34 sP 0?-R Ò9 4 Sa(Daewoo, RH-3550)u ó+

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(22) ! « :<. () PQR4 NO(400E550 C)q PQO(800 E1100 C) å O-R +,-., @t øÌù (F ?l ú' û} H>F ÞG +Ä Â ! AFG +,<. PQõ j]^ üý(Mullite, ID: 5 cm, L: 150 cm)u ;?+, -., þ O ÿ0# NO4 O Digital ThermometerR ÿ0+,9, PQO4 (# PQõ »O ö3+

(23) ¯ u 0ù Ç G +,<. NO 5M 4 PQ ÅF4 , 50% ì FG +,<. UVv34 STUV*-RZ HI { 4 ?a» : u V+,-., 1÷ Viù +4 4 2÷ Vi` VFG +,<. y ': @t^ Aspiratoru ?+

(24) L O/bcu ) -RZ P Qõ#

(25) (): UVFG +,<.

(26) . TPSZ ! ^ ðçÊÆ 2.5 wt%, 5.0 wt%, 7.5 wt%, 10.0 wt%1 s TPSZu +a ±+

(27) BCD?@# =>? @-R A+,<. Zr /øÜ F4 L^ ZrCl OÍ 8H O(Junsei, Japan, CP)u ;?+,-., Ti /ø Ü-R4 Ti[OCH(CH ) ] (Aldrich, USA, 99.999%)u ;?+,<. 2.5E10 wt% TiO U: TPSZ =>?@# þþ 600 C, 700 C, 800 C, 900 C, 1000 C, 1100 C $%&'()L TPSZ u +,<. J}9, þ N : 4 L b # A y , 110 C 3LWXY NL 2\# Å+,<.

(28) . : Â 4 W bª? ~# Æ·a ±+

(29) FT-Raman a(IFS120HR/FRA106A, Bruker, Germany)R b o. o. 4+. 2. 4+. 2. 3 2 4. 2. o. o. o. o. o. o. o. \# Å+,-., : b# 1 +a ±) XRD(MAC, MO3XHF, Japan)u ?+

(30) °± Scanning Speed: 5.00 deg/min 20 ≤2θ≤80 N-R iý# 9, à, cu ;+a ±) ¥;Ù!(SEM, Jeol, JSM5400, Japan) Ù!(TEM, Hitachi, H-7100, Japan) ;# <. y TPSZ ! ^ ICP-AES(JY 50P, Jobin Yvon, France)RZ \+,-., Áà _ U4 Particle Size Analyzer(Shimadzu, SA-CP3, Japan)R ÿ 0+,<. o. o.

(31) ï Â4 $%&'()*-R TPSZ i !u +,<. 4 9 2t1 a# 4

(32) jk{ +

(33) þ þ v¿# y iu A+4 Rë A * L Ç -., a å jku ¡[ù â+

(34) A+, i AoT ·<4 lg 3Û+9 U Ásy !u AÇ <. ï ñò4 ÈÉÊÆ Õ ðçÊ Æu ×+

(35) u A+,. 4 ÈÉÊÆ at1 ]# 6bLá4 Y 0 ÈÉÊÆu A+4Ó ?y o* F<. ÈÉÊÆ-ðçÊÆ at 1 ê 4 ! _» ðçÊÆ _ /Wt Ubc, ðçÊÆ _ à, àU bc ~ +., y ê {^ Lk A o* d è 56# §4<. STâ ) A: Lk4 ðçÊÆ _ U Ás+., -* ) AF4 Lk4 ðçÊÆ _ Kt Ásy U bcu x !Â Ás# +a 9, AK? bt-R Kí ¡¿ <. J x ï Â t?y $%&'()*-R Ay TPSZ4 Ás+9 ¢0]., Ý^ _ Uu 9 Â !Ä QV+ Þ4 9[ i !u <. XRD . Fig. 24 Ti þþ 2.5 wt%, 5.0 wt%, 7.5 wt%, 10 wt% FG +

(36) w 0.025 M ZrCl OÍ8H O/Ti[OCH(CH ) ] â ?@ # '()+

(37) y TPSZ i ! 2. 2. 3 2 4. Journal of the Korean Chemical Society.

(38)

(39) TPSZ . Fig. 2. X-ray diffraction patterns of as-prepared TPSZ powders by ultrasonic spray pyrolysis at 500 oC of drying zone and 1000 oC of pyrolysis zone prepared with 0.025 M Ti [OHC(CH3)2]4/ZrCl2O 8H2O aqueous solutions. (a: 2.5 wt%, b: 5.0 wt%, c: 7.5 wt%, d: 10 wt% in TiO2 content). y XRD iý# xç»<. J ! " y s TPSZ " y X# 2# $%·Ä, 2θì 30, 35.3, 50.5, 59, 60, 74.5 xçè &g}{ ÈÉÊÆ 2# xç»4 &g}{'# <. 4 TPSZ ( )*ù xçè PÄ, ðçÊÆ g4 &g}{ #+ Þ^Ó, JÔ^ ðçÊÆ ÈÉÊÆ K+

(40) bt-R ta ¯ ., &g}{ a4 ðçÊÆ H d H+,<. y <Ö y TPSZ pattern K) ï ¢, )*y ¢0 2# xç»4 ¬^ &g}{^ 800 C b : g + xç,-½R $%&'()* y TPSZ ! 4 800 Cb ty Ô-R ·1<. Raman . Fig. 34 0.075 M ZrCl OÍ8H O/ â?@# 800 C '() Ti[OCH(CH ) ] +

(41) Ay "Lku 3LW Ny ^ TPSZ " y Raman spectrau xç»<. J ·4 -q ¸ 147.1 cm , 275.6 cm , 312.8 cm , 456.9 cm , 647.6 cm xçè . 5M^ È o. o. 2. 2. o. 3 2 4. −1. −1. 2000, Vol. 44, No. 6. −1. −1. −1. 595. Fig. 3. Raman spectra of as-prepared TPSZ powders by ultrasonic spray pyrolysis at 400 oC of drying zone and 800 oC of pyrolysis zone prepared with 0.075 M Ti[OHC(CH3)2]4/ ZrCl2O 8H2O aqueous solutions. (a: 2.5 wt%, b: 5.0 wt%, c: 7.5 wt%, d: 10 wt% in TiO2 content). ÉÊÆ Tetragonal b y 2t1 &g}., c) iý 174 cm , 190 cm , 384 cm ±3 xçè Kt y a . &g}{^ ÈÉÊ Æ Monoclinic b )/+4 2 &g}'# <. 4 ÈÉÊÆ 800 C4 tetragonal b -R ¥R j+., ðçÊÆ 2.5E7.5%R bt-R Õs ¯ sO monoclinic b j# L;) ¥9 <. y monoclinic b# xç»4 2 &g}{ a4 ðçÊÆ Æ] G Õ+,<. Fig. 44 0.05 M ZrCl OÍ8H O/Ti[OCH(CH ) ] â?@# 1100 C '()+

(42) ^ 4 TPSZ "# y Raman spectrau xç0 Ô-RZ, a)iý# a1-R Ç ¯ 146.1 cm , 270.5 cm , 315.2 cm , 458.2 cm , 649.4 cm xçx 4 . &g}{^ ÈÉÊÆ Tetragonal b ) /+4 2t1 &g}., 177.5 cm , 189.3 1cm , 382.0 cm , 458.2 cm xçè . &g}{^ ÈÉÊÆ Monoclinic b 2t1 &g}u x ç0<. Fig. 3 Fig. 4u K)·Ä 800 C4 + õ2F Þ Monoclinic b 1100 C4 ) *+e xç3# -., y Ùb^ ðç ÊÆ bt-R t# ¯4 Kt + xç −1. −1. −1. o. 2. 2. 3 2 4. o. −1. −1. −1. −1. −1. −1. −1. −1. −1. o. o.

(43) . 596. Fig. 4. Raman spectra of as-prepared TPSZ powder by ultrasonic spray pyrolysis at the 500 oC of drying zone and 1100 oC of pyrolysis zone prepared with 0.05 M Ti[OHC(CH3)2]4/ ZrCl2O 8H2O aqueous solution. (a: 2.5 wt%, b: 5.0 wt%, c: 7.5 wt%, d: 10 wt% in TiO2 content at 1100 oC). ,-x, ðçÊÆ H d Monoclinic b ;4# ! <. y5 tetragonal b# x ç»4 . &g}{ m 270.5 cm q 315.2 cm å ó &g}u K)·Ä, ðçÊÆ b t-R t# ¯4 270.5 cm &g} a 6 7 -x, ðçÊÆ H d ¡&v8-R X+Ä J a ÕF4 PÄ, 315.2 cm . &g}4 v&v8-R X+Ä J a HF4 Ô-R xç,4Ó, 4 ðçÊÆq ÈÉ ÊÆ bª? Hy<4 Ô# xç0<. Fig. 54 ðçÊÆ ^ 2.5 wt%R s0+e å 9, q ) u ê L y TPSZ L k Raman spectrau xç0 Ô<. J ! " () HÇ G &g} a H+,4Ó, 4 HÇ G ¢0] K9 H+a ¯1 Ô-R þ:<. ê dÖ iý ê u $%·Ä, 800E 1000 C ;4 178 cm , 189 cm , 382 cm 458 cm O . &g}{^ + xçx Þ< 1100 C4 )*+e xç,4Ó, 4 TPSZ i ÈÉÊÆ Monoclinic b^ 1100 C b :<4 ;ñ# L;+9<. SEM TEM . Fig. 64 5 wt% ðçÊ Æ FG y TPSZ " SEM ;# −1. Fig. 5. Raman spectra of as-prepared TPSZ powder by ultrasonic spray pyrolysis at the various temperatures prepared with Ti[OHC(CH3)2]4/ZrCl2O 8H2O aqueous solution. (a: 800-0.075 M, b: 900-0.1M, c: 1000-0.025M, d: 1100-0.05M in 2.5 wt%). −1. −1. −1. −1. o. −1. −1. −1. o. o. Fig. 6. SEM photographs of as-prepared TPSZ powder by ultrasonic spray pyrolysis at 500 oC of drying zone and 1000 oC, 1100 oC of pyrolysis zone prepared with Ti[OHC (CH3)2]4/ZrCl2O 8H2O aqueous solution. Journal of the Korean Chemical Society.

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(45) TPSZ . 597. Fig. 7. TEM photographs of as-prepared TPSZ powder by ultrasonic spray pyrolysis at 500 oC of drying zone and 1000 oC, 1100 oC of pyrolysis zone prepared with Ti[OHC (CH3)2]4 /ZrCl2O 8H2O aqueous solution.. xç»<. : !{ _ à4 0.4E 0.8 µm 0R ª9 !+. O Â b# :9 4Ó, sO QVF 4 Ô _ r Ô J}9 _ ÃÄ ;] <= Ô# ! <. Ô^ Â @t U: ?l H> 4 a ) ) >+4 aU Â "»O !

(46) >? xz @+9 JR AB < H +Ä " »O C H+

(47) Â " r Ô-R þF., ;] <= Ô^ _ Dþ ¯ _ »O O ÷ dÖ ( EFG ÷R 1) ;] <= Ô ;k:<. y5 5 wt% ðçÊÆ FG y TPSZ " TEM ; H(ring pattern)# I u Fig. 7 xç»<. TEM ; ! " , : O "^ Â ., sO "^ O? þ-R F-x, J!x i g q4 } /X F Þ9 »O ËwF 4 Ô-R xç,<. y H# · Ä ï $%&'()*-R : !4 <¢ 0# 4<4 Ô# <. ICP . Table 14 ZrCl OÍ8H O/Ti[OCH 21. 2. 2000, Vol. 44, No. 6. 2. (CH ) ] â?@-ROr

(48) $%&'()*-R y TPSZ !u ¢KL Üo=*(ICP-AES)-R # \y ¢u xç»<. Ã ", Lk MR þ N3u «-RZ =>?@# A +9 $%&'()L ^ TPSZ !4 ñ ò Ü+4 R F4 ÞO-x P 0 s3+,<. . Table 24 $%&'()*-R þþ 1000 C 1100 C Ay TPSZ !{ Á_àu ðçÊÆ ê d xç »<. A: !{^ A # G _ U Ý9 Qy Â ! F-., ð çÊÆ TPSZ _{ à4 bõõ ª^ Ô-R xç,<. : TPSZ ! Á _ à4 0.65 µm,<. 3 2 4. o. o.

(49) $%&'()*-R ðçÊÆ # 2.5 wt% E10 wt%R ê LR TPSZ !{#

(50) .

(51) . 598. Table 1. ICP-AES data of TPSZ fine particles prepared by ultrasonic spray pyrolysis Ti contents(wt%) (800 oC-0.075M). Elements. 02.5 wt%. Ti /Zr. 16.1/728. 2.2/97.8. 05.0 wt% 07.5 wt% 10.0 wt%. Ti/Zr Ti/Zr Ti/Zr. 35.4/817 48.8/764 57.5/593. 4.2/95.8 6.0/94.0 8.8/91.2. (900-0.1 M) 02.5 wt% 05.0 wt% 07.5 wt% 10.0 wt%. Elements Ti/Zr Ti/Zr Ti/Zr Ti/Zr. Con. (ppm) 11.6/524 27.6/662 32.9/532 62.4/684. % 2.2/97.8 4.0/96.0 5.8/94.2 8.4/91.6. (1000 oC-0.025 M) 02.5 wt% 05.0 wt% 07.5 wt% 10.0 wt%. Elements Ti/Zr Ti/Zr Ti/Zr Ti/Zr. Con. (ppm) 19.4/1200 47.0/982 69.9/1070 101/891. % 5.1/94.9 4.6/95.4 6.1/93.9 10.2/89.8. (1100 oC-0.05 M) 02.5 wt% 05.0 wt% 07.5 wt% 10.0 wt%. Elements Ti/Zr Ti/Zr Ti/Zr Ti/Zr. Con. (ppm) 8.44/359.0 45.6/1020 82.9/1040 61.7/698.0. % 2.3/97.7 4.3/95.7 7.4/92.6 8.1/91.9. Con. (ppm). %. (unit: wt%) Table 2. Particle size distributions of TPSZ fine particles prepared by ultrasonic spray pyrolysis Ti contents Temp. o. 1000 C 1100 oC. 2.5 wt%. 5.0 wt%. 7.5 wt%. 10 wt%. Average. 0.3885 0.7362. 0.8923 0.7153. 0.4333 0.6082. 0.7442 0.7803. 0.6145 0.7100 (unit: µm). N +,-. J 2# ; +,<. $%&'()v34 ñòñ Aª +,-., $%& 'v34 sP 0? $%& S au ó+

(52) ;?+,<. PQõ 4 N 5 M^ 400E550 C, ()PQ 5M^ 850E1400 CR +,-., $%&' ) !y @t-R w{ Lk?@# mullite PQõ N, ()+

(53) ST UV*-R V+,<. 1) : ! 2^ =>BCD{ $a, () , $%& ' a, " V o* N ~ /0N {RZ Ç -., TPSZ !4 =>?@ S# G, P Qu eÇ G _U Ý9 Qy Â ! F<. o. o. !4 600 C + T^ 4 ¢0 ] ãU-., 800 C b 9 ¢0] i $!u AÇ <. 3) TPSZ i " ðçÊÆ 2.5E5.0 wt%1 °±4 ÈÉÊÆ tetragonal b ¥R õ2F-., ðçÊÆ btR ^ 7.5E10 wt%4 ÈÉÊÆ monoclinic b sO xç,9, y monoclinic b 2& g}{^ Æ] G H+,-.. 1100 C v )*+e xç,<. 4) y !4 SEM TEM ;-R ·Æ O Â-R »O Ë: $!R xç ,-., H# ·Æ <¢0# 4<4 Ô# 2) TPSZ. o. o. o. Journal of the Korean Chemical Society.

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(55) TPSZ . <. 5) $%&'()*-R y TPSZ "{^ 9s G _ U Ý9 Qy Â ! F-., : TPSZ ! Á _à4 0.65 µmR xç,<. ï Â4 ahOÍyVj¡ 0 Ú/)X÷OWahó>Ïr(CAPT) ¥T; 3#!X Ü y Ô_Ê<.. , ; : , 1994; p. 103. 2. ,

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(57) , 1977, 146, 55. 3. , , 1978, 13, 829. 1.. 4. Kim, D. J.; Kim, H. J. Kor. Ceram. Soc. 1989, 26(5), 691. 5. Roy, D. M.; Neurgaonkar, R. R.; Holleran, T. P. O.; Roy, R. Am. Ceram. Soc. Bull., 1977, 56(11), 1023. 6. Kanzaki, S.; Hirao, K.; Otsuka, N.; Saito, Z. YogyoKyokai Shi, 1983, 91(2) 81. 7. Lau, J. G. M. Am. Ceram. Soc. Bull., 1970, 56(11), 572. 8. Ruthner, M. J. Industrial Production of Multicomponent Ceramic Powders by Means of the Spray Roasting Technique in ceramic powders; Vincenzini, P., Ed.; Elsevier Scientific Publishing Co.: Amsterdam, Netherland, 1983; 515. 9. Lin, T. Q.; Sakurai, O.; Mizutani N.; Kato, M. J. Mat. Sci., 1986, 21, 3698.. 2000, Vol. 44, No. 6. 599. 10. Ishizawa, H.; Sakurai, O.; Mizutani, N.; Kato, M. K. Yogyo-Kyokai Shi, 1985, 93(7), 382. 11. Nogami, K.; Sakurai, O.; Mizutani N.; Kato, M. YogyoKyokai Shi, 1987, 95(7), 682. 12. Ishizawa, H.; Sakurai, O.; Mizutani, N.; Kato, M. Am. Ceram. Soc. Bull., 1986, 65(10), 1399. 13. Sakurai, O.; Mizutani N.; Kato M. Yogyo-Kyokai Shi, 1986, 94(8), 813. 14. Lang, R. J. J. Aconust. Soc. Am,. 1962, 34(1), 6. 15. Heuer A. H.; Hobbs, L. W. Advances in ceramic; Vol. 3, The American Ceramic Society: Columbus, U.S.A. 1981. 16. Garbie, R. C.; Hannink, R. H. J.; Urbani, C. Ceramurgia Int., 1980, 6(1), 19. 17. Hannink, R. H. J.; Johnston, K. A.; Pascoe R. T.; Garbie, R. C. Advances in ceramic; Heuer, A. H.; Hobbs, L. W., Eds.; The American Ceramic Society: Columbus, U.S.A., 1981; p. 36. 18. Lee, J. H.; Kim, B. H.; Choi, E. S.; Hwang, J. S. J. Kor. Ceram. Soc. 1993, 30(4), 325. 19. Cho, H. J.; Lee, J. H.; Park, S. J. J. Kor. Ceram. Soc. 1991, 28(11), 851. 20. Lee, J. H.; Cho, H. J.; Park, H. J. J. Kor. Ceram. Soc. 1991, 28(10), 831. 21. Cho, S. Y.; Lee, J. H.; Kim, M. C.; Park, S. J. J. Kor. Ceram. Soc. 1994, 31(5), 465. 22. Cho, S. Y.; Lee, J. H.; Park, S. J. Mater. Sci. 1995, 30(12) 23. Kim, B. H.; Lee, J. H. J. Kor. Ceram. Soc. 1994, 32(5), 575. 24. Ri, C. S.; Shim, I. S.; Kim, C. H.; Lee, B. K. Mat. Res. Symp. Proc. 1998, 520, 149..

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Synthesis and Characterization of Titania-Partially-StabilizedZirconia by Ultrasonic Spray Pyrolysis TPSZ 

Synthesis and Characterization of Titania-Partially-StabilizedZirconia by Ultrasonic Spray Pyrolysis TPSZ