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1 Jurnal f the Krean Ceramic Sciety Vl. 45, N. 5, pp. 285~289, Effect f Si:C Rati n Prsity and Flexural Strength f Prus Self-Bnded Silicn Carbide Ceramics Kwang-Yung Lim, Yung-Wk Kim, Sang-Kuk W*, and In-Sub Han* Department f Materials Science and Engineering, the University f Seul, Seul , Krea *Energy Materials Research Center, Krea Institute f Energy Research, Taejn , Krea (Received April 24, 2008; Accepted May 9, 2008) Si:C Ratiƒ œ Self-Bnded SiC»œ š e w Ÿ Á½ Á *Áw * w œw *w» l ( ; ) ABSTRACT Prus self-bnded silicn carbide (SiC) ceramics were fabricated at temperatures ranging frm 1750 t 1850 C using SiC, silicn (Si), and carbn (C) pwders as starting materials. The effect f the Si :C rati n prsity and strength was investigated as a functin f sintering temperature. It was pssible t prduce self-bnded SiC ceramics with prsities ranging frm 36% t 43%. The prus ceramics shwed a maximal prsity when the Si :C rati was 2 : 1 regardless f the sintering temperature. In cntrast, the maximum strength was btained when the rati was 5 :1. Key wrds : Prus ceramics, Silicn carbide, Self-bnded SiC, Prsity, Strength 1. œ ky³ (SiC) yw, ü, ü, w p w,» e w ƒ w,, p š» vl(diesel particulate filter), y» vl, vl, vl, š š, e f, š š. 1-5) œ SiC û ù { f j»ƒ j (grit) ƒw û w, ƒ 6) w š 2100 C š SiC y, š š w»œx 7) ƒw, s k s(fam) ky³ 8) gqw s k s w œ k y³ w, 9) 2,10) k y 11-13). Crrespnding authr : Yung-Wk Kim ywkim@us.ac.kr Tel : Fax : w œ SiC p»œ x, j»,»œ,»œ w œ» w p, q, w ü w p w. w p œ w. p SiC» w w j w. üy š vl ƒ w SiC w m w ky³ (clay-bnded SiC), f p w ky³ (silicate-bnded SiC), y³ w ky³ (silicn nitride-bnded SiC) y ky³ (recrystallized SiC). w ƒ, y ky³ y SiCƒ SiC wwš w» ƒ wù, ƒ 2100 C, 7) w š. m w ky³, f p w ky³ y³ w ky³ w w w SiC q ü y» w üy š vl ü š. wr, œ 285

2 286 Ÿ Á½ Á Áw Table 1. Batch Cmpsitin f Self-Bnded Silicn Carbide Ceramics Sample ky³ (prus reactin-bnded SiC (RBSC))» š, œ ky³ œ 2,10)»œ Si e w»œ»œ ƒ š, Si û w ü w š w š. 14) ky³ x (~ 65 µm) Si + C 20% ƒw Si + C w x SiC w w œ self-bnded SiC œ š w. p Si:C ratiƒ self-bnded SiC»œ š e w š w. w œ ƒ 1750 ~ 1850 C y ky³ 250 ~ 400 C û š š, SiC w w w w» ƒ w w š. w wz 2. x Batch Cmpsitin (wt%) SiC(#220) S Carbn Black ξ w SiC(~ 65 µm, > 98%, Shwa Denk, Tky, Japan), Si (< 1 µm, > 99%, High Purity Chemicals Ltd., Tky, Japan) C (~ 45 nm, > 99%, Krea Carbn Black C. Ltd., Krea). w Table 1, SB1 r w r SiC:(Si+C)=80:20 wt% š wš, Si:C rati 2:1 l 5:1¾ y g w. Table 1 w» w plyethylene glycl 6wt% ƒw SiC k w yww z, g. yw barxk ~31 MPa ƒ x w z 200 MPa x(cld isstatic pressing)w. x ƒ w 1750 C ~ 1850 C š» w 1 w., 1000 C ¾ 20 C/min w. r v l d w Remark SB SiC :(Si+C)=10 : 0 (wt%) SB SiC :(Si+ C)=8 :2 (wt%)/si: C =2 :1 (ml%) SB SiC :(Si+ C)=8 :2 (wt%)/si: C =3 :1 (ml%) SB SiC :(Si+ C)=8 :2 (wt%)/si: C =4 :1 (ml%) SB SiC :(Si+ C)=8 :2 (wt%)/si: C =5 :1 (ml%) ~65µm, > 98%, Shwa Denk, Tky, Japan <1µm, >99%, High Purity Chemicals Ltd., Tky, Japan ξ ~45 nm, > 99%, Krea Carbn Black C. Ltd., Inchn, Krea š,»œ l w. SiC g/cm 3 ƒ w. r CuKα w X- z (X-ray diffractin, XRD) ww š, r x (SEM, S-4300, Hitachi C., Japan) w w. r 10 mm 20 mm span w 4 š d 0.5 mm/min crss-head w ƒw d w. 3. š 3.1. Fig. 1 XRD z, Fig. 1(a) ky³ ƒw w r(sb1) Fig. 1(b) SiC : (Si + C) = 80 : 20 wt% š wš Si +C Si:C ratiƒ 5:1 r(sb5) 1850 C 1h w r. Fig. 1 r SiC. SB1 r Missanite (α-sic), 6H, 4H 3C (β-sic) š, SB5 r Missanite (α-sic), 6H 3C. w Fig. 1. X-ray spectra f prus self-bnded SiC ceramics sintered at 1850 C fr 1 h in Ar: (a) SB1 and (b) SB5 (refer t Table 1).

3 Si:C Rati가 다공질 Self-Bnded SiC 세라믹스의 기공율과 곡강도에 미치는 영향 SB5 시편에서는 2θ =43.333도에서 4H (JCPDS ) peak 및 2θ =75.562도에서 3C (JCPDS ) peak가 사라진 것을 관찰할 수 있는데, 이는 Si과 carbn이 반응 하여 SiC가 합성되면서 생긴 β-sic 상의 일부가 소결온 도에서 6H 상으로 상전이 하기 때문이다. 실제로 SB5 시 편에서 2θ =34.182도에서 6H (JCPDS ) 상의 peak 가 다소 높아진 것을 관찰할 수 있다(Fig. 1(b)). 한편 Yun 등에 의해 보고된 Si 침윤공정으로 제조된 다공질 RBSC 세라믹스의 경우에는 SiC peak 외에 잔류 Si의 peak가 상당히 강하게 남아 있는 것을 관찰할 수 있 는데, 이는 RBSC 공정의 특성상 Si의 침윤 공정을 정확 하게 제어하기 어렵기 때문이다. 그러나, Fig. 1(b)에서 보 듯이 본 연구에서 제조된 다공질 self-bnded SiC 세라믹 스는 Si:C rati가 5:1로 첨가됐음에도 불구하고, Si peak 가 전혀 발견되지 않았다. 이는 첨가된 Si과 C이 승온 도 중 및 소결온도에서 반응하여 SiC를 합성되고, 일부 과량 의 Si은 SiC 분말에 포함된 free carbn (~0.25 wt%)과 반응하여 SiC를 합성하며, 남은 과량의 Si은 소결온도가 1750~1850 C 범위로 다소 높으므로, 소결 도중에 기화하 여 흑연 도가니 등과 반응하기 때문이다. 실제로 흑연 도 가니 표면에는 기화한 Si과 반응하여 도가니의 표면이 SiC로 변한 것을 확인하였다. 14) 가 미세구조와 기공율에 미치는 영향 Fig. 2는 Si:C rati 변화에 따른 다공질 self-bnded SiC 세라믹스의 미세구조를 보여준다. 사진에서 보듯이 Si과 carbn의 반응에 의하여 합성된 5 µm 이하의 작은 SiC 입자가 형성된 것을 관찰할 수 있다. 이러한 작은 입 3.2. Si : C rati Fig 자들이 ~65 µm 크기의 대형 입자를 결합하고 있음을 알 수 있다. 기공 형성제를 사용하지 않았기 때문에 기공 형 성제에 기인하는 큰 기공은 관찰되지 않았으며, 기공의 크 기는 SEM 사진에서 관찰하였을 때 3~20 µm 범위였다. Si:C rati가 증가함에 따라 5 µm 이하의 입자의 수가 다 소 증가하였고, 기공크기는 변화가 없었다. Fig. 3는 온도 변화에 따른 다공질 self-bnded SiC 세라믹 스의 미세구조를 보여주는데, 출발원료로 SiC, Si 및 carbn 을 사용하여 1750~1850 C의 범위에서 소결한 결과, 소결온 도가 증가할수록 합성된 SiC 입자의 성장이 일어나 입자 크기가 5 µm 이하에서 10 µm까지 증가하는 모습을 관찰할 수 있으며, SiC의 입자 성장으로 인해 기공의 크기도 3~20 µm 범위에서 5~30 µm 범위로 다소 증가하였다. 입자 성자에 따른 기공 크기의 증가는 carbthermal reductin에 의해 제조된 다공질 SiC 세라믹스에서도 관찰되었다. Si:C rati와 소결온도를 제어 함으로서 제조한 다공질 self-bnded SiC의 기공율은 Fig. 4에서 보여주는데, 기공 율은 Si:C rati가 2:1일 때를 정점으로 Si의 비율이 높 을수록 기공율이 대체로 낮아지는 것을 알 수 있다. Si:C rati가 2:1일 때 기공율은 41-43%로서 가장 높았고, Si:C rati가 5:1일 때 기공율은 36-39%로서 가장 낮았다. 이 러한 결과는 Si:C rati가 증가함에 따라, 추가적인 치밀 화가 일어남을 의미한다. 기공율에 대한 소결온도의 영향은 일정한 관계를 나타 내지 않았는데, 이는 소결온도가 증가하면, 일반적으로 추 가적인 치밀화가 일어나려는 구동력과 Si 등의 기화 (vaprizatin)에 기인하는 밀도감소가 동시에 일어나며, 본 실험에서는 이러한 두 가지 현상이 어느 정도 균형을 이 15) Effect f the Si:C rati n micrstructure f prus self-bnded SiC ceramics sintered at 1850C fr 1 h in Ar: (a) SB1, (b) SB2, (c) SB3, and (d) SB5 (refer t Table 1). 제 45 권 제 5호(2008)

4 임광영 김영욱 우상국 한인섭 288 Fig. 3. Effect f sintering temperature n micrstructure f prus self-bnded SiC ceramics cntaining 20 wt% Si and C in 5 : 1 mlar rati: (a) 1750C, (b) 1800C, and (c) 1850C. 루어서 소결온도가 기공율에 미치는 영향이 명확하게 나 타나지 않았다고 생각된다. Si:C rati가 2:1이고, 소결온도가 1850 C일 때, 최대 기 공율 43%가 얻어졌고, Si:C rati가 5:1이고, 소결온도가 1850 C일 때 최소 기공율 36%가 얻어졌다. 본 실험에서 는 Si:C rati와 소결온도를 제어 함으로서 다공질 selfbnded SiC의 기공율을 36~43% 범위에서 제어하는 것이 가능하였다. 가 강도에 미치는 영향 Fig. 5는 Si:C rati와 소결온도에 따른 self-bnded SiC 3.3. Si : C rati Fig. 4. Effects f the Si : C rati and sintering temperature n prsity f prus self-bnded SiC ceramics. 한국세라믹학회지 세라믹스의 곡강도의 변화를 보여준다. 다공질 self-bnded SiC 세라믹스의 곡강도는 Si:C rati가 증가함에 따라 증 가하였고, 소결온도의 변화에 따라서는 큰 영향을 받지 않았다. 이러한 결과는 Fig. 2에서 보여주듯이 Si:C rati 가 증가함에 따라 5 µm 이하의 입자의 수가 다소 증가한 결과와 일치하며, Si과 carbn의 반응에 의해 형성된 5 µm 이하의 SiC 입자가 ~65 µm 크기의 대형 SiC 입자를 결합 하여 강도를 부여함을 알 수 있다. 또한 소결온도의 변화 에 따라 강도 값에 의미 있는 변화를 보여주지 않는데, 이 는 Fig. 4에서 보듯이 소결온도의 변화에 따라 기공율에 서 의미 있는 변화가 나타나지 않는 결과와 일치한다. Fig. 5. Effects f the Si : C rati and sintering temperature n flexural strength f self-bnded SiC ceramics.

5 Si:C Ratiƒ œ Self-Bnded SiC»œ š e w 289 œ SiC»œ w w. x 4,16) selfbnded SiC w w ùkþ, C œ self-bnded SiC»œ Si:C ratiƒ 2: % ƒ š, Si : C ratiƒ ƒw w. œ self-bnded SiC Si:C rati ƒ 5:1 18 MPa ƒ š, Si:C ratiƒ w w. w œ selfbnded SiC sw Si:C rati»œ w w ùkü. Si:C ratiƒ 5:1 š, 1750 C»œ 39% self-bnded SiC š ~18 MPa ƒ ƒ š ù kþ. w š Se 10) šw Si e œ w»œ 36% œ RBSC š 18 MPa w ù, Si e œ w»œ 36% œ RBSC free Si w wš š, x w self-bned SiC XRD Si peak d š q. 4. (~ 65 µm) SiC Si carbn w, Si carbn w w 5µm w SiC ƒ ~65 µm j» x SiC wwš œ self-bnded SiC 1750 ~ 1850 C w. œ self-bnded SiC»œ Si:C rati ƒ 2: % ƒ š, Si:C ratiƒ ƒ w w. œ self-bnded SiC Si:C ratiƒ 5:1 18 MPa ƒ š, Si:C ratiƒ w w. Si:C rati w œ self-bnded SiC»œ 36~43% w ƒ w. Acknwledgment (the Ministry f Knwledge Ecnmy)» w. REFERENCES Esturnes, and J. Guille, Influence f the Preparatin Cnditins n the Synthesis f High Surface Area SiC fr Use as a Hetergeneus Catalyst Supprt, J. Mater. Sci., (1999). 2. S.-S. Hwang and T.-W. Kim, Fabricatin and Prperties f Reactin Bnded SiC Ht Gas Filter Using Si Melt Infiltratin Methd, J. Kr. Ceram. Sc., 40 [9] (2003). 3. J. Adler, Ceramic Diesel Particular Filters, Int. J. Appl. Ceram. Technl., 2 [6] (2005). 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. Y.-W. Kim, Y. S. Chun, T. Nishimura, M. Mitm, and Y. H. Lee, High-Temperature Strength f Silicn Carbide Ceramics Sintered with Rare-Earth Oxide and Aluminum Nitride, Acta Mater., 55 [2] (2007). 6. S. H. Kim, Y.-W. Kim, J. Y. Yun, and H. D. Kim, Fabricatin f Prus SiC Ceramics by Partial Sintering and their Prperties(in Krean), J. Kr. Ceram. Sc., 41 [7] (2004). 7. V. Z. Stavric and M. Hue, Rekristallisiertes Siliziumkarbid, Keram. Zeit., 27 [3] (1975). 8. S. H. Kim and Y.-W. Kim, Prcessing f Cellular SiC Ceramics Using Plymer Micrbeads, J. Kr. Ceram. Sc., 43 [8] (2006). 9. F. F. Lange and K. T. Miller, Open Cell, Lw-Density Ceramics Fabricated frm Reticulated Plymer Substrates, Adv. Ceram. Mater., 2 [4] (1987). 10. K. S. Se, S. W. Park, and H. B. Kwn, Fabricatin f Prus RBSC by Si Melt Infiltratin, J. Kr. Ceram. Sc., 37 [11] (2000). 11. Y.-W. Kim, S. H. Kim, I. H. Sng, H. D. Kim, and C. B. Park, Fabricatin f Open-Cell, Micrcellular Silicn Carbide Ceramics by Carbthermal Reductin, J. Am. Ceram. Sc., 88 [10] (2005). 12. 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). 13. J. H. Em, Y.-W. Kim, and M. Narisawa, Micrstructural Develpment f Macrprus Silicn Carbide ceramics During Annealing, J. Ceram. Prc. Res., 9 [2] (2008). 14. S. H. Yun, P. N. Tan, Y. D. Kim, and S. W. Park, Effects f Amunts f Carbn Surce and Infiltrated Si n the Prsity and Fracture Strength f prus Reactin Bnded SiC, J. Kr. Ceram. Sc., 44 [7] (2007). 15. J. H. Em, Y.-W. Kim, I. H. Sng, and H. D. Kim, Micrstructure and Prperties f Prus Silicn Carbide Ceramics Fabricated by Carbthermal Reductin and Subsequent Sintering Prcess, Mater. Sci. Eng. A, (2007). 16. J. H. Em, Y.-W. Kim, I. H. Sng, and H. D. Kim, Prcessing and Prperties f Plysilxane-Derived Prus Silicn Carbide Ceramics Using Hllw Micrspheres as Templates, J. Eurp. Ceram. Sc., (2008). 1. N. Keller, C. Pham-Huu, S. Ry, M. J. Ledux, C. 45«5y(2008)

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