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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 1, pp. 35~40, Effects f Template Size and Cntent n Prsity and Strength f Macrprus Zircnia Ceramics Su-H Chae, Yung-Wk Kim, In-Hyuck Sng*, Hai-D Kim*, and Ji S Bae** Department f Materials Science and Engineering, the University f Seul, Seul , Krea *Pwder Materials Research Divisin, Krea Institute f Materials Science, Changwn , Krea **Yung-Jin Ceramics C., Ltd, Chnnam , Krea (Received Octber 23, 2008; Accepted January 14, 2009)»œx j» w œ g»œ e w yá½ Á x*á½w *Á ** w œw * (KIMS) **( ) ( ; ) ABSTRACT Using zircnia and ply (methyl methacrylate-cethylene glycl dimethacrylate) (PMMA) micrbeads, macrprus zircnia ceramics were fabricated by a simple pressing methd. Effects f template size and cntent n micrstructure, prsity, and flexural and cmpressive strengths were investigated in the prcessing f the macrprus zircnia ceramics. Three different sizes f micrbeads (8, 20, and 50 µm) were used as a template fr fabricating the macrprus ceramics. The prsity increased with increasing the template size at the same template cntent. The flexural and cmpressive strengths were primarily influenced by the prsity rather than the template size. Hwever, the strengths increased with decreasing the template size at the same prsity. By cntrlling the template size and cntent, it was pssible t prduce macrprus zircnia ceramics with prsities ranging frm 58% t 75%. Typical flexural and cmpressive strength values at 60% prsity were ~ 30 MPa and ~ 75 MPa, respectively. Key wrds : Prus ceramics, Zircnia, Template, Prsity, Strength 1. œ»œ j», x, w»œ œ» w, q, w ü w w. w ƒ œ 1-8)»œj»»œ w œ w v. œ g w ü w üy,, š. w, yw ü w ey w Crrespnding authr : Yung-Wk Kim Tel : Fax : š. œ g 9,10) ƒ œ š. œ g œ j (replica), lv p(template) (partial sintering) ù. š s g gqwš, w š ƒ w»œ x w. lv p 11) e (carbn), l 12), š 13) 14) g w Ì yww x w z, l v p w k»œ x w. Gain 12) lv p e ƒw (multi-pass) œ w w œ g w. wr, g x ù w, ü»œ û œ g w 35

2 36 yá½ Á xá½w Á Table 1. Sample Designatin and Batch Cmpsitin f Macrprus ZrO 2 Ceramics Sample Batch cmpsitin (wt%) Remark ZrO 2 PMMA 8 µm PMMA 20 µm PMMA 50µm PMMA cntent (vl%) PZ PZ PZ PZ PZ PZ PZ PZ PZ PZ PZ PZ ƒ» x 15) k. g» 16) œx azdicarbnamide yw jš, x(die) œ ƒ û t ù œ g w. wr, w œ g w» w 20 µm j» s PMMA w š, z 8µm 17) 50 µm j» s ƒ PMMA w»œ sƒ œ g»œ e w š w. 18) ƒ j» s ƒ PMMA w»œx j»(8, 20, 50 µm) w (50, 60, 65, 70 vl%) yƒ œ g,»œ» e w š w. w wz 2. x üy ZrO 2 (ZC7F7, Universal America, Inc., USA) PMMA (ply(methyl methacrylate-cethylene glycl dimethacrylate, ~ 8 µm, ~ 20 µm ~50 µm, Sigma-Aldrich Inc, St. Luis, MO) w. xœ w plyethylene glycl plyvinyl alchl ƒƒ 2% ƒw. w Table 1, lv p 8 µm, 20 µm 50 µm j» PMMA w š, w 50 ~ 70 vl% y g 12ƒ w w. yw w, ZrO 2 s v v w (ball milling) w. yw z œ e z, 40 mm 8mm 5 mm j» r 50 MPa ƒ x w š, 120 MPa þ ƒ x(cld isstatic pressing, CIP)w. x» w œ»» 3 C/min t ¾ ƒ w w. ƒƒ 1550 C 2 š w. r v (bulk density, D b ) (g) v(v) l w. D b (g/cm 3 )=M(g)/V(cm 3 ) (1)»œ (P) v (D th ) ƒ š w w. P(%)=(1 D b /D th ) 100 (2) œ g x (SEM, S-4300, Hitachi C., Japan) w w š, š x»(instrn 4461, Nrwd C., USA) w d w. (σ cmpressive ) 0.5 mm/min crss-head w ƒ w w w. σ cmpressive (Pa) = F (N) / (d 1 (m) d 2 (m)) (3)» F q w, d 1, d 2 w r ƒ ¼ ùkü. š ü span 10 mm, span 20 mm e w 0.5 mm/min crss-head 4 š d w. 3. š Fig C 2 w r, 8 µm PMMA 50 vl% ƒw œ g r

3 기공형성제 크기와 함량이 다공질 지르코니아 세라믹스의 기공율과 강도에 미치는 영향 Fig. 1. Fig Typical micrstructures f macrprus zircnia ceramics sintered at 1550C fr 2 h in air: (a) PZ8-50 and (b) PZ50-70 (refer t Table 1). Effect f PMMA cntent n the micrstructure f macrprus zircnia ceramics sintered at 1550C fr 2 h in air: (a) PZ8-50, (b) PZ8-60, (c) PZ8-65, and (d) PZ8-70 (refer t Table 1). (PZ8-50)과 50 µm PMMA를 70 vl% 첨가한 시편(PZ5070)의 파단면을 보여준다. PMMA 미세구의 함량과 크기 가 서로 다른 두 시편이지만, 소결온도와 시간이 같기 때 문에 지르코니아 입자의 크기나 입자간의 결합 정도는 큰 차이를 보이지 않았다. 하지만 PMMA 미세구 함량 및 크 기가 50 vl%, 8 µm에서 70 vl%, 50 µm로 변함에 따라, 기공 크기는 10~20 µm에서 20~60 µm으로 커졌고, 기공 율은 58.4%에서 75.0%로 증가했다. Fig. 1의 기공구조는 기공형성제로 첨가된 PMMA 미세구가 볼 밀링 및 성형 공정에서 손상되지 않고, 소결 공정에서 PMMA의 분해 온도까지 구형 형상을 유지했음을 나타낸다. 또한 다공질 지르코니아 세라믹스의 기공 크기 및 기공율을 제어하기 위해서는 PMMA 미세구의 크기 및 함량의 제어가 중요 함을 나타낸다. Fig. 2는 소결조건을 1550 C/2h으로 고정하고, 8 µm 크 기의 미세구 함량을 변화시켜 제조한 다공질 지르코니아 세라믹스의 파단면을 보여준다. 첨가 된 8 µm PMMA 미 세구의 함량이 50, 60, 65, 70 vl%로 증가함에 따라, 기 공율은 각각 58.4, 61.2, 63.2, 66.2%로 증가하였다. 미세 조직을 살펴보면 PMMA 미세구의 함량이 50%에서 70% 로 증가함에 따라 기공 크기가 8~20 µm에서 10~60 µm 로 증가하였고, 기공의 형상이 구형에서 불규칙적인 형상 으로 변한 것을 알 수 있다. 이러한 대형 기공의 형성은 8 µm PMMA 미세구의 함량이 증가함에 따라 서로 접촉 할 수 있는 기회가 많아져, 미세구가 응집되어서 생긴 기 공이다. 따라서, PMMA 미세구의 함량이 60 vl% 이상일 경우에는 이러한 대형 기공의 형성을 방지하기 위해, 미 세구와 지르코니아 분말의 균일한 혼합이 매우 중요함을 알 수 있다. Fig. 3은 소결조건 및 PMMA 미세구의 함량을 각각 1550 C/2 h 및 50 vl%로 고정하고, 미세구의 크기를 변화 시켜 제조한 다공질 지르코니아 세라믹스의 파단면을 보 제 46 권 제 1호(2009)

4 채수호 김영욱 송인혁 김해두 배지수 38 Fig. 3. Effect f PMMA size n the micrstructure f macrprus zircnia ceramics sintered at 1550C fr 2 h in air: (a) PZ8-50, (b) PZ20-50, and (c) PZ50-50 (refer t Table 1). 여준다. 첨가한 PMMA 미세구의 크기가 8 µm, 20 µm, 50 µm으로 커짐에 따라, 각각의 기공 크기는 8~20, 20~30, 50~60 µm로 증가하였고, 기공율도 58.4, 63.3, 73.3%로 증가하였다. 선행연구에서는 동일함량의 이중 크 기 분포를 갖는 PMMA 미세구(8 µm 및 50 µm)를 첨가하 였을 때 50 µm 크기의 미세구 비율이 높아질수록 기공율 이 증가하였다. 따라서 이러한 현상은 50 µm 크기의 대 형 PMMA 미세구의 첨가로 형성된 기공은 소결 공정 동 안에 확산(diffusin)에 기초한 치밀화 공정으로 제거되기 어려우나, 8 µm 크기의 PMMA 미세구에 의해 형성된 기공 은 소결 공정 동안에 기공의 일부가 치밀화 되어 전체적인 기공율이 낮아지는데 기여한다고 판단된다. 결국 다공질 지 르코니아 세라믹스의 기공율은 같은 함량의 미세구를 첨가 하더라도, 미세구의 크기가 증가함에 따라 증가함을 알 수 있다. 이러한 결과는 미세구의 크기를 제어하는 것도 기공 율 제어의 한가지 방법일 수 있다는 것을 나타낸다. Fig. 4는 PMMA 미세구의 함량에 따른 다공질 지르코 니아 세라믹스의 기공율 변화를 보여준다. 8 µm 미세구를 첨가한 시편은 58.4~66.2% 범위의 기공율을 나타냈고, 20 µm 및 50 µm PMMA 미세구를 첨가한 시편은 각각 63.3~68.6% 및 73.3~75.0% 범위의 기공율을 나타냈다. 소결조건(1550 C/2 h)과 PMMA 미세구의 크기가 동일 할 때 첨가된 기공형성제 함량이 증가함에 따라 기공율이 증 가하는 경향을 나타냈다. 이러한 경향은 PMMA를 기공 형성제로 첨가한 다공질 SiC 및 다공질 뮬라이트 (mullite) 세라믹스에서도 관찰되었다. 또한, 소결조건과 PMMA 미세구의 함량이 동일 할 때 첨가된 기공형성제 18) 의 크기가 증가함에 따라 기공율이 증가하였다. 상기 결 과는 소결조건(1550 C/2 h)이 고정되었을 때 PMMA 미세 구의 함량과 크기를 제어함으로써 다공질 지르코니아 세 라믹스의 기공율 58~75%의 범위에서 제어하는 것이 가 능함을 나타낸다. Fig. 5는 1550 C에서 2시간 동안 소결한 시편의 기공형 성제 함량 변화에 따른 곡강도 및 압축강도의 변화를 보 여준다. Fig. 5에서 보듯이 PMMA 미세구의 함량이 증가 할수록, 또한 미세구의 크기가 증가할수록 곡강도 및 압 축강도가 감소하는 경향을 나타냈다. 8 µm 미세구를 첨 가한 시편이 전 범위에서 가장 높은 강도를 나타냈고, 3,19) 20) 한국세라믹학회지 Fig. 4. Prsity f macrprus zircnia ceramics sintered at 1550C fr 2 h in air as a functin f template cntent.

5 »œx j» w œ g»œ e w 39 Fig. 5. Strength f macrprus zircnia ceramics sintered at 1550 C fr 2 h in air as a functin f template cntent: (a) flexural strength and (b) cmpressive strength. Fig. 6. Strength f macrprus zircnia ceramics sintered at 1550 C fr 2 h in air as a functin f prsity: (a) flexural strength and (b) cmpressive strength. 8 µm 50% ƒw r š ƒƒ ~37 MPa ~97 MPa š, 60% ƒw r ~29MPa š ~78MPa ù kþ. wr, 50 µm PMMA ƒw r w ƒ š yƒ š, w 5~6 MPa š 8~15MPa ùkþ. 50 µm PMMA ƒ œ g ü 50 ~ 60 µm j»»œ x gš,» œ w w,»œ y ƒ. š»œ š w» w Fig. 5»œ w ùkü š, Fig. 6. Fig. 6,»œ ƒ x š, œ g š»œj»»œ ƒw w w ù kþ. w œ g š»œ j»ƒ 10 ~ 60 µm,»œj»»œ w. w œ š ƒ»œ w w w. 17) wr, Gain 12) 70 nm j» ZrO ~ 200 µm j» PMMA w œ g w š, œ g š»œ 53%, š ƒ 150 MPa w. Fig. 5 mw PMMA j»ƒ œ g 46«1y(2009)

6 40 yá½ Á xá½w Á w, Gain œ g š» w PMMA j» g j» w w w ùkü. ù j», w k v w š q. 4. j»ƒ 3ƒ PMMA»œx w x 1550 C 2 w»œ»œj»ƒ œ g w. PMMA w w, œ g»œ»œx j»ƒ ƒw ƒw š, PMMA j»ƒ w»œx w ƒw ƒw., PMMA j» w w œ g»œ 58 ~ 75% w ƒ w. ù» œ œ g š»œx j» w ƒw w. œ g š»œ 65% ƒƒ ~20MPa ~50MPa. Acknwledgment 21» v p» y x» (the Center fr Advanced Materials Prcessing, CAMP) w,. REFERENCES 1. Y. P. Jin and Y. T. Chu, Thermal and Mechanical Prperties f Prus Y-PSZ/Zircn Cmpsites, Mater. Res. Innvat., (1998). 2. J. W. Baek and D. J. Kim, Ceramic Fams by the Self- Blwing f Plymer (in Krean), J. Kr. Ceram. Sc., 41 [7] (2004). 3. S. H. Lee and Y.-W. Kim, Prcessing f Cellular SiC Ceramics Using Plymer Micrbeads, J. Kr. Ceram. Sc., 43 [8] (2006). 4. J. H. Em, D. H. Jang, Y.-W. Kim, I. H. Sng, and H. D. Kim, Lw Temperature Prcessing f Prus Silicn Carbide Ceramics by Carbthermal Reductin (in Krean), J. Kr. Ceram. Sc., 43 [9] (2006). 5. D. H. Jang, K. Y. Lim, and Y.-W. Kim, Effects f Additive Cmpsitin and Cntent n Sintered Density and Cmpressive Strength f Crdierite Ceramics (in Krean), J. Kr. Ceram. Sc., 44 [4] (2007). 6. J. H. Em and Y.-W. Kim, Fabricatin f Silicn Oxycarbide Fams frm Extruded Blends f Plysilxane, Lw- Density Plyethylene (LDPE), and Plymer Micrbead, Met. Mater. Int., 13 [6] (2007). 7. B. H. Yn, E. J. Lee, H. E. Kim, and Y. H. Kh, Highly Aligned Prus Silicn Carbide Ceramics by Freezing Plycarbsilane/Camphene Slutin, J. Am. Ceram. Sc., 90 [6] (2007). 8. Y.-W. Kim, J. H. Em, C. Wang, and C. B. Park, Prcessing f Prus Silicn Carbide Ceramics frm Carbn- Filled Plysilxane by Extrusin and Carbthermal Reductin, J. Am. Ceram. Sc., 91 [4] (2008). 9. C. Heisel, M. Silva, and T. P. Schmalzried, Bearing Surface Optins fr Ttal Hip Replacement in Yung Patients, J. Bne. Jt. Surg., 85 [7] (2003). 10. G. Dell Agli, S. Espsit, G. Mascl, M. C. Mascl, and C. Pagliuca, Films by Slurry Cating f Nanmetric YSZ (8 ml% Y 2 O 3 ) Pwders Synthesized by Lw-Temperature Hydrthermal Treatment, J. Eur. Ceram. Sc., 25 [12] (2005). 11. I. K. Jun, Y. H. Kh, J. H. Sng, S. H. Lee, and H. E. Kim, Imprved Cmpressive Strength f Reticulated Prus Zircnia Using Carbn Cated Plymeric Spnge As Nvel Template, Mater. Lett., (2006). 12. A. K. Gain and B. T. Lee, Micrstructure Cntrl f Cntinuusly Prus t-zro 2 Bdies Fabricated by Multi-Pass Extrusin Prcess, Mater. Sci. Eng. A, (2006). 13. B. Nait-Ali, K. Haberk, H. Vesteghem, J. Absi, and D. S. Smith, Thermal Cnductivity f Highly Prus Zircnia, J. Eurp. Ceram. Sc., (2006). 14. A. K. Gain, H. Y. Sng, and B. T. Lee, Micrstructure and Mechanical Prperties f Prus Yttria Stabilized Zircnia Ceramic Using Ply Methyl Methacrylate Pwder, Scripta Mater., (2006). 15. Z. Y. Deng, J. F. Yang, Y. Beppu, M. And, and T. Ohji, Effect f Agglmeratin n Mechanical Prperties f Prus Zircnia Fabricated by Partial Sintering, J. Am. Ceram. Sc., 85 [8] (2002). 16. X. Yang, Z. Xie, and L. Wang, Fabricatin f Prus Zircnia Ceramics by Injectin Mlding Methd, Key Eng. Mater., (2008). 17. S. H. Chae, J. H. Em, Y.-W. Kim, I. H. Sng, H. D. Kim, J. S. Bae, S. M. Na, and S. I. Kim, Prsity Cntrl f Prus Zircnia Ceramics (in Krean), J. Kr. Ceram. Sc., 45 [1] 65-8 (2008). 18. S. H. Chae, Y.-W. Kim, I. H. Sng, H. D. Kim, and J. S. Bae, Effect f Template Size Rati n Prsity and Strength f Prus Zircnia Ceramics (in Krean), J. Kr. Ceram. Sc., 45 [9] (2008). 19. J. H. Em and Y.-W. Kim, Effect f Template Size n Micrstructure and Strength f Prus Silicn Carbide Ceramics, J. Ceram. Sc. Jpn, 116 [10] (2008). 20. Y.-W. Kim, H. D. Kim, and C. B. Park, Prcessing f Micrcellular Mullite, J. Am. Ceram. Sc., 88 [12] (2005). w wz

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