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1 Jurnal f the Krean Ceramic Sciety Vl. 47, N., pp. 18~188, 010. DOI: /KCERS Preparatin f Ce 0.8 Gd 0. O 1.9 Pwder by Milling f CeO Slurry and Oxalate Precipitatin S-Man Sim Schl f Materials Science and Engineering, Hngik University, Chungnam 0-701, Krea (Received Nvember 5, 009; Revised January 8, 010; Accepted January 5, 010) CeO e w Ce 0.8 Gd 0. O 1.9 w y w œw ( ; ; ) ABSTRACT Ce 0.8 Gd 0. O 1.9 (GDC0) pwder was synthesized by milling f CeO slurry and Gd xalate precipitatin. The mixture f CeO pwder and Gd precipitates calcined at 600 C fr h shwed the particle size distributin similar t that f CeO pwder, which had been milled during the synthesis prcess. Attritin milling f the calcined pwder with an average particle size f 0.6 µm fr h resulted in a decrease in the particle size t 0.4 µm. Althugh the milled pwder cnsisted f small particles(<1 µm), a small amunt f fine platy Gd O particles, which had been survived in the milling prcess, was bserved. Sintering f the pwder cmpacts fr 4 h shwed relative densities f 80.7% at 100 C and 97% at 1400 C, respectively. Densificatin was fund t almst cmplete at 1500 C, resulting in a dense and hmgeneus micrstructure with a relative density f 99.5%. Key wrds : SOFC, GDC, Oxalate precipitatin, Milling, Sinterability 1. ZrO (YSZ) Gd v CeO (GDC) Y O y ƒ» x š y (IT-SOFC) w ƒÿ š. ù 1,) e yƒ Ce Gd y yww w y yw š GDC š (>1500 C) w w.,) e w w w» w y e, 4,5) e, 6-10) citrate, 11,1) glycine-nitrate 1,14) w w w CeO wš. e e w ƒ ûš, w û, š x ƒ w ƒ. e e w w f w ƒ. Zhang 9) Ce Gd e w w Crrespnding authr : S-Man Sim smsim@hngik.ac.kr Tel : Fax : GDC0(Ce 0.8 Gd 0. O 1.9 ) 5 w ƒ e w w. w j»ƒ z w w 1150 C ~98% ù, w ~9% w š w. Han 10) GDC0 e w wš w 100 C 97.4% š tw. Maca 15) CeO Gd O ywwš 48 ¾ w w, ~6 ƒ ƒ w 1550 C 98% ù w w š w. w x wš j» w w, w w w w ù w ƒ. e w»ƒ š w z w vwš CeO wš Gd y e g GDC0 (Ce 0.8 Gd 0. O 1.9 ) w wš, e w x, w p, w. 18

2 184. x GDC0 w w CeO (99.9%, Junsei), 0.5M Gd (Gd(NO ) 6H O, 99.9%, Aldrich) 0.5M (C H O 4 H O, 99%, Aldrich) w. Gd 1.5 ƒ + wš ph 6.5 w. CeO ZrO ball(ø mm) attritin jar š, w w yw. 500 rpm ƒ k Gd w e ù w. e ph 6.5 wš, 1 w. CeO Gd e ƒ w, filter press(0. µm, Millipre) w wš k k w z 80 C 1 w. 600 C w w z, k ywwš attritin mill w. r w w (0.5 wt%, PVB, Aldrich) ƒwš, 50 MPa ƒ w 15 mm pellet x k xw 00 MPa þ x (cld isstatic press) w. r 600 C w w wš 1000~1500 C 4 œ» ww. CeO Gd e yw w TG/DTA(TG-DTA 000, MAC Science) w 5 C/min œ» 100 C¾ wš, Gd e w w. w w 400~1000 C w w XRD(CuK α, M0XHF, MAC Science) wš, r wì w. r Archimedes d wš, GDC0 (7. g/cm ) l w. 10) z»(sald-001, Shimadzu) d wš, x r SEM(FE- SEM, JEOL) w.. š Fig. 1(a) CeO Gd e yw e TG/DTA š, e CeO wì Gd e w ùkùš. ph 6.5 w Gd e y (NH 4 Gd(C O 4 ) H O). 6) peak(11 C) k w ~5% ƒ š, k z Fig. 1. TG/DTA curves f (a) a mixture f CeO pwder and Gd precipitate, and (b) Gd precipitates. w y» w peak(54 C, 47 C)ƒ ùkû. e CeO ƒ w Gd e w w 17.% w, ~700 C l yƒ e w Gd O w. Fig. 1(b) Gd e TG/DTA š, Fig. 1(a) w w. k w peak(15 C, 194 C) w y w peak(400 C, 566 C)ƒ, y Fig. 1(a) óùš 50.1% (50.9%) ew. Fig. e w w XRD pattern. w w (as-prepared) XRD pattern CeO z peak Gd e w w w z peakƒ wì. e w Ce Gd e e w š ù, 10) e Gd e ùkû. w 400 C CeO z peak w w w, w ƒ ƒw j w w wz

3 CeO 슬러리 분쇄와 옥살산 침전을 이용한 Ce Gd O 분말의 합성 185 Fig.. XRD patterns f GDC sintered at 100 C and 1400 C fr 4 h. Fig.. XRD patterns f GDC pwders calcined at varius temperatures( : Gd precipitate). 것으로 보아 CeO 분말 입자들은 하소온도에서 결정성장 이 거의 일어나지 않음을 알 수 있다. 또한 회절강도가 큰 Gd O 회절 peak들은 CeO 회절 peak와 일치하고 Gd O 가 소량 존재하기 때문에 모든 하소온도에서 CeO 회절 peak만이 관찰되었다. Fig. 은 100 C, 1400 C에서 각각 4시간 소결한 시편 의 XRD 회절 pattern으로서 1000 C에서 하소한 분말 보 다는 강도가 큰 CeO 회절 peak를 보여주고 있으며, 각 각의 회절 peak에 면지수가 함께 표시되어 있다. 소결온 도가 높아지면 회절 peak의 강도도 점차 증가하므로 결 정상이 잘 발달하였음을 알 수 있다. Ce와 Gd가 잘 혼합 되어 있는 공침물은 하소과정에서 고용체가 형성될 수 있 지만, 산화물을 혼합한 경우에는 1600 C에서 Gd이 완전 히 고용된다고 알려져 있다. 본 연구에서 하소한 분말에 는 Gd 침전물의 열분해에서 생성된 미세한 Gd O 입자 가 CeO 분말과 함께 존재하므로 산화물 혼합법보다는 낮 은 온도에서 Gd가 고용될 수 있어 소결시편의 회절 peak 는 GDC에 해당하는 것으로 판단된다. 분말합성에 사용된 CeO 분말의 분쇄특성을 조사하기 ) Fig. 4. Particle size distributins f (a) attritin-milled CeO, and (b) calcined and attritin-milled GDC pwders. 위해 attritin mill로 1시간 동안 분쇄하고 입도분석을 하 였다. Fig. 4(a)는 평균 입경이 4. µm인 CeO 분말을 각 제 47 권 제 호(010)

4 심수만 186 Fig. 6. Relative densities and pen prsities f the samples sintered fr 4 h at varius temperatures. 큰 입자들이 모두 없어지고 평균 입경도 0.4 µm으로 약 간 감소하였다. Fig. 5(a)는 600 C에서 하소한 GDC0 분말의 SEM 사 진으로서 합성한 분말과 거의 동일한 입자 크기와 형상 을 보여준다. 하소 분말에는 옥살산 침전에서 판상 형태 로 생성되는 Gd 침전물이 분말합성 과정에서 모두 분쇄 되지 않고 약간 남아 있는 것이 관찰되었다. 분쇄한 분말 은 Fig. 5(b)에서 보듯이 하소 분말에 있던 판상 입자들이 대부분 분쇄되었고, 1 µm보다 훨씬 작은 입자들로 이루 어져 있었다. Fig. 5(c)의 고배율 사진을 보면 큰 판상 입 자가 분쇄되면서 1 µm보다 작은 판상 입자로 일부 남아 있는 것이 발견되었다. 또한 이들 분말 입자들은 Gd O 로 보이는 매우 작은 구상의 입자들과 CeO 입자들이 서 로 응집되어 있었으며, 합성과정에서 분쇄된 것으로 보이 는 각상 형태의 CeO 입자들도 함께 존재하고 있었다. 입 자 형상으로 보아서는 600 C의 낮은 하소온도에서 Gd O 는 CeO 에 거의 고용되지 않을 것으로 판단된다. Fig. 6은 1000~1500 C에서 4시간 소결한 시편의 밀도와 개기공률을 나타낸 것이다. 소결은 1000 C에서는 거의 일 어나지 않아 성형밀도와 비슷한 57.7%의 밀도를 나타내 었으며 1000 C와 100 C 사이에서는 치밀화가 느리게 일 어나서 밀도는 완만히 증가하였다. 그러나 100 C에서부 터는 치밀화가 급속히 일어나서 100 C에서 80.7%인 밀 도는 1400 C에서 97%에 달하였고, 이와 함께 100 C에 서 1%인 개기공률도 1400 C에서 0.1%로 급감하였다. 치 밀화는 1500 C에서 거의 완료되어 밀도는 99.5%로 약간 증가하였고 개기공률도 더 이상 변화가 없었다. GDC0 분말의 소결성은 본 연구의 합성법 보다 비교 적 복잡한 옥살산 침전법으로 제조한 분말보다 못하지만 산화물 혼합법에 비하면 훨씬 우수한 것으로 나타났다. Ma 등 은 ~0.5 µm 입경의 CeO 와 Gd O 분말로 제조한 GDC0의 밀도는 1600 C에서 97% 이상이었으나, 100 C Fig. 5. SEM micrgraphs f GDC pwders: (a) calcined at 600 C and (b) and (c) calcined and attritin-milled fr h. 각 0분, 60분씩 분쇄한 후의 입도 변화를 보여준다. 분 쇄하기 전 분말에 70% 정도 존재하였던 1~0 µm 크기의 입자들은 1시간 동안 분쇄한 후에는 대부분 사라지고 평 균 입경은 0. µm으로 감소하였으며, 분말의 85%가 1 µm 보다 작은 입자들로 되어 있었다. Fig. 4(b)는 600 C에서 하소하고 시간 동안 분쇄한 GDC0 분말의 입도분포이 다. 하소한 GDC0 분말은 평균 입경이 0.6 µm으로 입 도분포가 Fig. 4(a)의 1시간 분쇄한 CeO 분말과 거의 비 슷하므로 분말합성 과정에서 CeO 분말이 분쇄되었음을 나타내고 있다. 분쇄한 후의 GDC0 분말에는 1 µm 보다 한국세라믹학회지 )

5 CeO 슬러리 분쇄와 옥살산 침전을 이용한 Ce Gd O 분말의 합성 187 건식 분쇄하여 각각 100 C, 1400 C에서 본 연구에서의 밀도보다 높은 95%, 98%의 밀도를 얻었다. Zhang 등 은 옥살산 침전법으로 제조한 GDC 분말을 하소하고 planetary mill로 5시간 건식 분쇄하여 1150 C에서 ~98%의 밀도를 얻었으며, Han 등 도 GDC0 분말을 attritin mill로 시 간 습식 분쇄하여 100 C에서 97%의 밀도를 얻었다고 보 고하였다. Fig. 7(a)는 100 C에서 소결한 시편의 SEM 사진으로 서, 입자들이 합체하여 결정립이 형성되기 시작하고 불규 칙한 형태의 많은 기공들이 입자 사이에 존재하고 있었 다. 어둡게 나타난 부분은 소결이 빨리 진행되어 미세구 조가 치밀한 부분으로 소결 초기단계를 약간 지나서 치 밀화가 시작되고 있음을 의미한다. 소결온도 1400 C에서 는 Fig. 7(b)에서처럼 치밀화가 빠르게 진행되어 밀도가 97%에 달하였으며, 많은 기공들이 폐기공으로 변하였다. 결정립들은 대부분 0.5 µm 보다 작은 크기로 분포되어 있 으며, 이들 결정립이 합체하여 ~ µm까지 성장한 결정립 들도 함께 관찰되어 입성장이 진행되고 있는 것으로 보 인다. Fig. 7(c)는 1500 C에서 소결한 시편으로서 기공이 거의 없는 치밀하고 균일한 미세구조가 형성되었고, 잘 발달된 결정립과 입계가 뚜렷이 나타났다. 그러나 입성장 은 급속히 일어나서 결정립은 ~8 µm까지 성장하였다. 결 정립 형태로 보아 입성장은 거의 끝나고 결정립의 조대 화가 일어나기 시작함을 알 수 있다. 9) 10) 4. 결 론 슬러리의 분쇄와 동시에 옥살산 용액으로 Gd 수 화물을 침전시켜서 Ce Gd O 분말을 합성하였다. Gd 침전물과 CeO 분말 혼합물을 600 C에서 시간 하소하 여 분말합성 과정에서 분쇄된 CeO 분말과 비슷한 입도 분포를 지닌 평균 입경 0.6 µm인 분말을 얻었다. 하소분 말을 시간 분쇄한 결과, 평균 입경은 0.4 µm로 약간 감 소하였고 분말은 모두 1 µm보다 작은 입자들로 구성되었 으며, 이들 입자 중에는 판상의 Gd O 입자들도 소량 존 재하였다. 분말의 소결성은 산화물 혼합법 보다는 우수하 여 100 C에서 80.7%인 밀도는 1400 C에서 97%에 달하 였다. 치밀화는 1500 C에서 거의 완료되어 밀도가 99.5% 인 치밀하고 균일한 미세구조가 형성되었다. 입성장은 1400 C와 1500 C 사이에서 급속히 일어나서 1400 C에서 0.5 µm 보다 작은 결정립들이 1500 C에서 ~8 µm까지 성 장하였다. CeO Fig. 7. SEM micrgraphs f the samples sintered at (a) 100 C, (b) 1400 C, and (c) 1500 C fr 4 h. 에서는 7%로 본 연구의 밀도 80.7% 보다 낮았다. Trrens 등 도 입경이 ~0. µm인 GDC0 분말로 1650 C에서 98% 의 밀도를 얻었으나, 1400 C에서는 본 연구의 밀도 97% 보다 훨씬 낮은 86%에 불과하였다. 최근 기계화학적 합 성을 이용하여 GDC0 분말을 제조한 Maca 등 은 각각.7 µm,. µm 입경의 CeO, Gd O 분말을 attritin mill 로 ~6시간 동안 습식 분쇄하여 1550 C에서 98% 이상의 밀도를 얻었다고 하였다. 반면에 옥살산 침전법으로 CeO 계 분말을 만든 Higashi 등 과 Herle 등 은 하소 분말을 7) 15) 8) 6) Acknwledgment 본 연구는 007학년도 홍익대학교 학술연구진흥비의 지 원으로 수행되었으며, 이에 감사드립니다. 제 47 권 제 호(010)

6 188 REFERENCES 1. H. Inaba and H. Tagawa, "Review Ceria-Based Slid Electrlytes, Slid Sate Inics, (1996).. V. V. Khartn, F. M. Figueired, L. Navarr, E. N. Naumvich, A. V. Kvalevsky, A. A. Yaremchenk, A. P. Viskup, A. Carneir, F. M. B. Marques, and J. R. Frade, Ceria-Based Materials Fr Slid Oxide Fuel Cells, J. Mater. Sci., (001).. J. Ma, T. S. Zhang, L. B. Kng, P. Hing, and S. H. Chan, Ce 0.8 Gd 0. O -δ Ceramics Derived Frm Cmmercial Submicrn-Sized CeO and Gd O Pwders fr Use as Electrlytes in Slid Oxide Fuel Cells, J. Pwer Surces, (004). 4. J.-G. Li, T. Ikegami, Y. Wang, and T. Mri, 10-ml%- Gd O -Dped CeO Slid Slutins via Carbnate Cprecipitatin: A Cmpartive Study, J. Am. Ceram. Sc., 86 [6] (00). 5. A. I. Y. Tk, L. H. Lu, and F. Y. C. Bey, Carbnate Cprecipitatin f Gd O -Dped CeO Slid Slutin Nan- Particles, Mat. Sci. & Eng., A8 9-4 (004). 6. J. V. Herle, T. Hrita, T. Kawada, N. Sakai, H. Ykkawa, and M. Dkiya, Oxalate Cprecipitatin f Dped Ceria Pwder fr Tape Casting, Ceram. Internatinal, (1998). 7. R. S. Trrens, N. M. Sammes, and G. A. Tmsett, Characterisatin f (CeO ) 0.8 (GdO 1.5 ) 0. Synthesised Using Varius Techniques, Slid State Inics, (1998). 8. K. Higashi, K. Snda, H. On, S. Sameshima, and Y. Hrata, Synthesis and Sintering f Rare-Earth-Dped Ceria Pwder by Oxalate Cprecipitatin Methd, J. Mater. Res., 14 [] (1999). 9. T. S. Zhang, J. Ma, L. B. Kng, P. Hing, Y. J. Leng, S. H. Chan, and J. A. Kilner, Sinterability and Inic Cnductivity f Cprecipitated Ce 0.8 Gd 0. O -δ Pwders Treated via a High-Energy Ball-Milling Prcess, J. Pwer Surces, (00). 10. I.-N. Dng, K.-Y. Lim, and S.-M. Sim, Preparatin and Sintering Characteristics f Gd-Dped CeO Pwder by Oxalate C-Precipitatin(in Krean), J. Kr. Ceram. Sc., 4 [10] (006). 11. R. A. Rcha and E. N. S. Muccill, Physical and Chemical Prperties f Nansized Gadlina-Dped Ceria Prepared by the Catin Cmplexatin Technique, Mater. Res. Bull., (00). 1. R. O. Fuentes and R. T. Baker, Structural, Mrphlgical and Electrical Prperties f Gd 0.1 Ce 0.9 O 1.95 Prepared by a Citrate Cmplexatin Methd, J. Pwer Surces, (009). 1. X. Guan, H. Zhu, Y. Wang, and J. Zhang, Preparatin and Prperties f Gd + and Y + C-Dped Ceria-Based Electrlytes fr Intermediate Temperature Slid Oxide Fuel Cells, J. Allys and Cmpunds, (008). 14. L. D. Jadhav, M. G. Churashiya, K. M. Subhedar, A. K. Tyagi, and J. Y. Patil, Synthesis f Nancrystalline Gd Dped Ceria by Cmbustin Technique, J. Allys and Cmpunds, (009). 15. Maca, J. Cihlar, K. Castkva, O. Zmeskal, and H. Hadraba, Sintering f Gadlinia-Dped Ceria Prepared by Mechanchemical Synthesis, J. Eur. Ceram. Sc., (007). w wz

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