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1 Jurnal f the Krean Ceramic Sciety Vl. 45, N. 11, pp. 681~687, Effects f Sr n the Characteristics f PZT Ceramics Prepared by Hydrthermal Prcess Bem-Sek Yang, Chang Yun Shin, and Chang Whan Wn Engineering Research Center fr Rapidly Slidified Materials, Chungnam Natinal University, Daejen , Krea (Received July 11, 2008; Revised September 2, 2008; Accepted September 2, 2008) w w PZT p e Sr w Á Á y û w š ( ; ; ) ABSTRACT The sintering and electrical prperties f the hydrthermal PSZT pwders btained by substituting 4, 6 and 8 ml% Sr fr Pb in PZT lattice structure were investigated. The lattice cnstant and particle size decreased in prprtin t a quantity f Sr. The sintering prperties f PSZT pwders shwed g/cm 3 f sintered density and 4 µm f grain size at sintering temperature f 1250 C. Curie temperature lwered gradually frm C t C and relative dielectric cnstants increased rapidly by a quantity f Sr. In cmparisn t PZT, mrever, the quality factr f PSZT was increased mre than three times with increase f Sr mle rati, and piezelectric cnstant (d 31 and g 31 ) was decreased. It was fund that dielectric lss f PSZT was decreased by 0.574% which was half f PZT. Key Wrds : Pb(Zr 0.52 Ti 0.48 )O 3, Hydrthermal prcess, piezelectric element, PSZT 1.» Ÿw p j ƒ š, thin film z»q p p y, š,, Ÿ, Ÿ z. w p w {, DRAM, thin film g, t k q»q,, Ÿ q e, Ÿ, v š. w Ÿ PbZr 1-x Ti x O 3 (PZT)»» p j š 1,2). PZT PbTi 0.48 Zr 0.52 O 3 (rhmbhedral) (tetragnal) ƒeƒ. MPB (mrphtrpic phase bundary) š p ùkü. MPB PZT p (piezelectric transducer) š. w»» y w x Crrespnding authr : Chang Whan Wn cwwn@cnu.ac.kr Tel : Fax : j š. w», q l, l š w ƒ ƒ w, w w š. x ƒ PZT 1951 Shirane w 1954 Jaffe 3,4) w Zr/Ti = 58/ 42 (Mrphtrpic Phase Bundary, MPB) w. Isupv 5) single phase plarizatin dmain rientatin j ù» š w, 6,7) w ƒ. x ƒ š š 8), ƒ jš w yw ƒ û ƒ j»ƒ ƒw mw j» w., ƒ. w t» w 99.9% yw ³ p w j»,, s š» 681

2 682 Á Á y Table 1. Specificatins f the Raw Materials Used in Hydrthermal Synthesis f PZT Pwders Cmpnents Frmula Manufacturer Purity Pb precursr Pb(CH 3 COO) 2 H 2 O Junsei chemical C., Ltd Min. 99.5% Ti precursr TiO 2 Degussa (30~50 nm) Min. 99.8% Zr precursr ZrOCl 2 H 2 O Junsei chemical C., Ltd Min. 90.0% Mineralizer KOH Samchun chemical C., Ltd Min. 85.0% Dpant SrCl 2 Junsei chemical C., Ltd Min. 98.0% ƒ ƒ w» v w. Jaffe Ck 9) PZT» Pb Sr Ca e m eywš Nb, Ta, Cr, La, Fe m y ƒw ùkü»-» w (Electrmechanical cupling factr, K) (ε) š» w sft- PZT w w. ù PZT» p w p y ƒ w j w» Dnr ù Acceptr ƒ p 3 r e px w ƒ v w. 2+ w w 10) 2+ Pb Sr eyw PSZT wš p» p y wš w. 2. x ZrOCl 2 H 2 O, TiO 2, š Pb Pb(CH 3 COO) 2 H 2 O w š, Ÿy KOH w. TiO 2 j» 30 ~ 50 nm anatase x DEGUSSA w w. x p Table 1 ùkü š Alkali m Sr 2+ (1.27 Å) Pb 2+ (1.32 Å) ey j» w r Table 2 ùkü. x w» Fig. 1 ùkü. w» ü vessel tefln w š, impeller w y w» w Nickel w. w magnetic drive impeller e cntrller w w. ü vessel 1 liter š vessel il bath heater w. Fig. 2 PZT œ ùkü. Pb Zr, Ti e w z š 1 w w ƒƒ yk w. TiO 2 yk ZrOCl 2 8H 2 O yww yw wš yw lead ww, x v w dpant wì yww yw w. yw e w y w» w tefln beaker KOH x ƒw, KOH ƒ w ph y w» w k ww. Ÿy n yw 11) w» wš x, w w g. z vessel ü ƒ 80 C w ü kƒ w ph 7.5 wƒ ¾ w š œ» 24 w. ƒ x XRD (SIEMENS, Mdel:D5000) w. X-ray Table 2. Cmpsitin fr Dping Experiment At% Dpant A site B site Pb Sr Zr Ti Sr Fig. 1. Schematic diagram f hydrthermal reactr. w wz

3 수열합성법에 의해 제조된 PZT의 특성에 미치는 Sr의 영향 683 Fig. 3. XRD patterns f Sr dped PZT pwders at varius Sr ml rati. (a) 0 ml%l, (b) 4 ml%, (c) 6 ml%, (d) 8 ml% 간 유지 후 750 C에서 30분간 열처리하였다. 압전특성 측 정을 위한 분극은 120 C 절연유 속에서 3 kvdc/mm로 15 분간 실시하였다. 유전특성 및 압전특성은 Digital LCR multimeter (TERASYSTEM사, MIT1216A)와 Impedance/ gain phase analyzer (HP사, HP4194A)를 사용하여 측정하 였다. Fig. 2. Flw chart f experimental prcedure f hydrthermal synthesis. 가속전압은 40 kv, 30 ma이었다. 주사 속도는 0.05 /sec이 었고, X-선의 target으로는 Cu를 사용하였다. 생성물의 미 세구조를 관찰하기 위하여 SEM (JEOL사, Mdel:JSM5410)을 사용하였다. 전기적 특성을 측정하기 위한 소결 체 제조를 위해 약 350 Mpa의 압력으로 성형하여 10 mmφ 의 원판형 시편을 제조하였으며, 얻어진 소결체는 #1200 SiC 연마지로 두께가 동일하도록 연마하였다. 소결체의 전 기적 특성측정을 위한 전극처리는 시편의 양쪽표면에 Ag cver paste (DS-7178TR)를 silk screen하여 400 C에서 30분 3. 결과 및 고찰 Fig. 3에 위의 실험 조성식에 따라 Sr의 몰비를 4, 6 그 리고 8 mle%씩 치환하여 제조한 PSZT분말의 XRD patterns를 나타내었다. Sr을 도핑하지 않은 (a)의 PZT peak 와 비교해 보면 주 peak인 (101), (110)면의 intensity는 Sr 의 치환량이 늘어날수록 감소하였고 Sr이 도핑된 후 오 른쪽으로 이동한 것을 알 수 있다. 그리고 (002)T, (200)T 및 (200)R면을 확대하여 나타낸 (b)를 보면, Sr의 치환량 증가에 따라 서서히 (200)R면의 intensity가 증가하는 것 을 알 수 있다. 이것은 정방정상과 능면정상의 분율이 Sr 의 도핑에 의해 변화하고 있음을 나타내며 Sr의 도핑에 의해 상경계영역의 위치변화가 가능함을 의미한다. Zheng 제 45 권 제 11호(2008)

4 양범석 신창윤 원창환 반경이 1.27 Å으로써 가장 큰 원인은 이온반경 차이인 것 으로 사료된다. 이처럼 PZT계에 있어서 grain size와 유전 특성의 상관관계에 대한 연구결과가 특정시점(1970년대) 을 기준으로 상이한 이유는 사용된 시약의 정제기술의 차 이에 의해 일어나는 실험적인 오차 때문인 것으로 판단 된다. 압전재료의 전기적 특성은 grain size 1~10 µm의 범 위에서는 grain size와 비례관계에 있다는 것이 정설로 받 아들여지고 있다. 다른 연구결과들과 동일한 결과로써 PZT의 전기적인 특성들이 grain bundary에 축적된 space charge의 생성에 의해 영향을 받는다. 유전재료의 경우 grain bundary는 내부에 비해 낮은 저항을 가지게 되어 동일한 직류전계 하에서 높은 누설전류를 보이고, 국부적 Fig. 4. Dependence f the lattice cnstant and lattice anistrpy 인 항복(lcal breakdwn) 또는 고착된 charge carrier에 의 f Pb1-xSrx(Zr0.52Ti0.48)O3 ceramics n the amunt f 한 field-assisted emissin이 잘 일어나게 된다. 그러므로 Sr additives. 상변태 도중 grain bundary로 산소공공과 같은 공간전하 등 과 Csta 등 은 Sr을 각각 32 mle%와 30 mle%까 들이 축적되게 되며, grain bundary의 전위장벽이 높아지 지 치환시킨 결과 정방정상에서 pseudcubic상으로의 상 게 된다. 이때 축적된 공간전하들로 인해 전자 전도를 위 변화가 관찰되었다고 하였으나, 본 실험의 치환 몰비 범 한 활성화 에너지가 낮아져 grain bundary로 전류가 더 위에서는 이러한 상변화는 관찰되지 않았으며, 근소하게 쉽게 흐르게 되며 누설전류는 grain bundary의 수가 증 가함에 따라 증가하게 된다. 능면정상의 분율이 높아지는 것을 알 수 있었다. Fig. 5에 Sr의 치환 몰비에 따라 제조된 PSZT 분말의 Fig. 4에 Sr의 치환량에 따른 격자상수를 계산하여 그 림으로 나타내었으며 치환량이 늘어남에 따라 c/a가 감소 SEM 사진을 나타내었다. Sr의 치환량이 4 mle%일 경우 하고 있는 것을 알 수 있다. 여기에서 a값은 거의 변화가 입자크기 2 µm ~4 µm의 분산된 분말을 얻을 수 있었고 없거나 오히려 Sr 치환량 증가에 따라 약간 증가하였으 6 mle%와 8 mle%로 Sr의 치환량이 늘어나면서 근소하 나 c값의 감소로 인하여 c/a가 감소하는 결과를 나타내었 게 입자크기가 작아지는 경향을 보였다. 도핑 몰비의 증 다. 그 이유는 Pb 의 이온반경이 1.32 Å이고 Sr 의 이온 가에 따라 입자의 크기가 작아지는 현상은 PZT에 몇 가 ) 13) Fig. 5. SEM phtgraphs f Sr dped PZT pwders synthesized by hydrthermal prcess at varius Sr ml rati. (a) 4 ml%, (b) 6 ml%, (c) 8 ml% 한국세라믹학회지

5 수열합성법에 의해 제조된 PZT의 특성에 미치는 Sr의 영향 685 Fig. 6. SEM phtgraphs f 6 ml% Sr dped PZT sintered bdy at varius sintering temperature. (a) 1000 C, (b) 1100 C, (c) 1250 C, (d) 1300 C 지 다른 금속산화물이 혼입될 때에도 관찰되는 현상 이 며 이는 격자 내에 크기가 다른 이온이 혼입됨에 따라 입 자의 성장이 억제되기 때문이라고 사료된다. Fig. 6에 Pb Sr (Zr Ti )O 분말을 온도별로 소결 하여 관찰한 SEM 사진을 나타내었고, Fig. 7에는 각각의 Sr 치환량에 따른 소결체의 밀도 및 소결체의 두께 변화 를 온도별로 나타내었다. SEM 사진으로부터 1250 C에서 소결 시 grain size는 1~4 µm의 크기로 불균일하나 기공 이 없는 소결체를 얻을 수 있었다 C에서는 PbO가 소결체 내부로부터 휘발하여 소결체의 표면에 응고된 것 을 관찰할 수 있다. 이는 같은 온도로 소결한 PZT에서는 관찰되지 않던 현상으로 치환된 Sr이 소결 조제의 역할 을 일부 수행함으로써 도핑 되지 않았을 때 보다 Pb의 휘 발이 더욱 가속화되었기 때문이라고 사료된다. 그러나 8 mle%까지의 Sr 치환에 의한 저온소결 즉, PZT보다 상대 적으로 낮은 온도에서의 소결은 이루어지지 않았다. Fig. 8 에 나타낸 온도에 따른 밀도의 변화에 따르면 Sr의 치환 량 변화에 따른 밀도의 큰 변화는 관찰되지 않았으며 Fig. 7. Temperature dependence f the density and thickness f Fig. 8. Temperature dependence f the dielectric cnstant f 14) sintered bdy f the hydrthermal PSZT with varius Sr cntents. the hydrthermal Pb1-xSrx(Zr0.52Ti0.48)O3 with varius Sr cntents. 제 45 권 제 11호(2008)

6 686 Á Á y Table 3. Variatin f Prperties in the Hydrthermal PZT with Sr Replacing a Prtin f Pb Cmpsitin Sintering Density (g/cm 3 ) Dielectric cnstant tan δ k p (%) d 31 (10 12 C/N) g 31 (10-3 Vm/N) Q m Tc ( C) Pb(Zr 0.52 Ti 0.48 )O Pb 0.96 Sr 0.04 (Zr 0.52 Ti 0.48 )O Pb 0.94 Sr 0.06 (Zr 0.52 Ti 0.48 )O Pb 0.92 Sr 0.08 (Zr 0.52 Ti 0.48 )O mle% ƒ. ƒ 90% ü w pre w p w ¾. PZT ƒ 8.14 g/cm % ùk ü ü w»œ w q j w. grain size w y w ù q. š w grain bundary w space charge w j w w œ, 1 p w w ü w š q. PSZT ƒ ƒ w Pb ƒ. ƒ 1250 C 1300 C Pb { ƒ w q. Pb ƒ Pb { ƒ p ùkü ¾ j w e q. Fig. 8 y Sr ey p d w ùkü. Sr ƒ C, 346 C š C û, Sr ey ƒ ƒƒ , , Sr ey PZT C 989 w Sr ey j s w jš j z ƒ. w PZT w Sr ey ƒ» t 3 ƒw d31 g31 w. wr (tanδ) ey ƒ 8mle% 0.574%¾ w z ƒ»» w Sr ey w j. PZT PSZT p p Table 3 w ùkü. w wz 4. w w PSZT wš p sƒ w w. w Sr ƒƒ 4, 6, 8 ml% PZT ü e yw PSZT wš p w» p d w. Sr ey w j»ƒ w C grain sizeƒ 4µm š ƒ g/cm, ey ƒ C C û š ƒw. w PZT w Sr ey ƒ» t 3 ƒw d 31 g 31 w. wr (tanδ) ey ƒ 8mle% 0.574%¾ w z ƒ»» w Sr ey w j. REFERENCES 1. H. Haertling, Ferrelectric Ceramics: Histry and Technlgy, J. Am. Ceram. Sc., 82 [4] (1999). 2. E. K. Akdgan, M. R. Lenard, and A. Safari, Size Effects in Ferrelectric Ceramics, pp , Handbk f Lw and High Dielectric Cnstant Materials and Their Applicatins Academic Press, Lndn, New Yrk, and San Dieg, D. Berlincurt, H. H. A. Krueger, and B. Jaffe, Stability f Phases in Mdified Lead Zircnate with Variatin in Pressure, Electric Ffield, Temperature, and Cmpsitin, J. f Physics and Chemistry f Slids, 25 [7] (1964). 4. B. D. Dianv and A. G. Kuz-menk, Investigatin f the Ppssibilities fr Bradening the Transmissin Band f Cylindrical Piezelectric Ceramic Transducers, Ultrasnics, 9 [2] 123 (1971). 5. V. A. Isupv, Cmments n the paper X-ray Study f the PZT Slid Slutins Near the Mrphtrpic Phase Transitin, Slid State Cmmunicatins, 17 [11] (1975). 6. C. I. Chen and H. G. Kim, Effects f Chemical Inh-

7 w w PZT p e Sr w 687 mgeneity n Phase Cexistence in Pb(Zr,Ti)O 3 Ceramics at Mrphtrpic Tetragnal and Rhmblhedal Phase Bundary(in Krean), J. Kr. Ceram. Sc., 27 [8] (1990). 7. B. B. Kim, B. S. Yang, K. S. Yun, and C. W. Wn, The Effect f Reactin Parameters in the Characteristic f PZT Pwders Synthesized by SHS(in Krean), J. Kr. Ceram. Sc., 42 [5] (2005). 8. M. H. Lee, I. C. Wang, W. K. Ch, and B. H. Lee, Study n the Develpment f Piezelectric Ceramics(in Krean), J. Kr. Ceram. Sc., 15 [3] (1978). 9. B. Jaffe, W. R. Ck, and H. Jaffe, Piezelectric Ceramics, J. Sund and Vibratin, 20 [4] (1972). 10. E. A. Delikuras and D. D. Perlmutter,, J. Am. Ceram. Sc., 77 [12] (1994). 11. Y. Deng, L. Liu, Y. Cheng, C. Nan, and S. Zha, Hydrthermal Synthesis and Characteristics f Nancrystalline PZT Pwders, Materials Letters, (2003). 12. H. Zheng, I. M. Reaney, W. E. Lee, N. Jnes, and H. Thmas, Effects f Strntium Ssubstitutin in Nb-dped PZT Ceramics, J. Eur. Ceram. Sc., (2001). 13. C. E. F. Csta, F. M. Pntes, A. G. Suza, E. R. Leite, P. S. Pizani, and E. Lng, Influence f Sstrntium Cncentratin n the Structural, Mrphlgical, and Electrical Prperties f Lead Zircnate Titanate Thin Films, Appl. Phys., A (2004). 14. P. Ry-Chwdhury and S. B. Dwshpande, Effect f Dpants n the Micrstructure and Lattice Parameters f Lead Zircnate-Titanate Ceramics, J. Mater. Sci., (1985). 45«11y(2008)

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