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1 Jurnal f the Krean Ceramic Sciety Vl. 47, N. 6, pp. 546~55, 010. DOI: /KCERS Micrstructure and Permeability Prperty f Si Bnded Prus SiC with Variatins in the Carbn Cntent In-Hyuck Sng, Mi-Jung Park, Hai-D Kim, Yung-Wk Kim*, and Ji-S Bae** Engineering Ceramics Grup, Krea Institute f Materials Science, Changwn , Krea *Department f Materials Science and Engineering, The University f Seul, Seul , Krea **YJC C. Ltd., Chnnam , Krea (Received Octber 10, 010; Revised Octber 6, 010; Accepted Octber 8, 010) Si w œ ky³ m» p - e w y x Á Á½w Á½ *Á ** * w œw **( ) ( ; ; ) ABSTRACT The achievement f high gas permeability is a key factr in the develpment f prus SiC ceramics fr applicatins f ht gas filter, vacuum chuck, and air spindle. Hwever, few reprts n the gas permeability f prus SiC ceramics can be fund in the literature. In this paper, prus SiC ceramics were fabricated at temperatures ranging frm 1600 C t 1800 C using the mixing pwders f SiC, silicn, carbn and brn as starting materials. In sme samples, expanded hllw micrspheres as a pre frmer were used t make a cellular pre structure. It was pssible t prduce Si bnded SiC ceramics with prsities ranging frm 4% t 55%. The maximum bending strength was 58 MPa fr the carbn cntent f 0. wt% and sintering temperature f 1700 C. The increase f air permeability was accelerated by additin f hllw micrsphere as a pre frmer. Key wrds : SiC, Prus ceramics, Permeability, Prsity 1. œ 15~95%»œ e,» e w ƒ w p ( :,, ) w» e w š. p œ» j (1) ü»œ (pen pre, penetrating pre) w filtratin/ separatin z () ü»œ/s»œ j», x, w,»œ, s w» ƒ w p w w.»œ p w ƒ š, š e (kiln furniture), k,,, üy, š ƒ vl(ht gas filter), y vl(water filter), Crrespnding authr : In-Hyuck Sng sih1654@kims.re.kr Tel : Fax : ,, w v s (prefrm) w 1-3) ƒ w. w œ y w» w w. p w» w ùƒ»œ w p m» w. m» w œ w vl š ù, m» w LCD»q ƒ v wš w» w œ w ƒ wš. ky³ (SiC) t š» p ü y, ü, ü, w, l š. p œ w w SiC w p wš ù. û ƒ ƒ wš z x e xk wš ky³ (RBSC, Reactin 546

2 Si w œ ky³ m» p -e w y 547 Bnded Silicn Carbide)ƒ š. 4-7) w ¾ œ ky³ vl wš, œ (1) m(clay)» w (inrganic binder) w š ky³ w g œ ky³, () ³ œ x en j ù y ³ e gq ky³ œ x en g ³y ky³ x g š œ ky³, (3) ky³ w yw» š ky³ x e g ky³ w w œ k y³. p œ ky³ (RBSC, Reactin Bnded Silicn Carbide)» SiC e x Si e g RBSC 1800 C š Si g œ RBSC w». ù œ Si e 8-11) j»»œ x œ w» w œ ww š, w š Si j œ w. w œ ky³ œ wš ryw» w Self-Bnded SiC(SBSC) œ š. 1,13) w» p w m» ƒ ƒ œ SiC w» w w SiC w»œ(pen pre) x gš, Si SiC w g œ SiC wš w. p y e w y» p y»œ p y š w. w m» w j» w œ x ƒw ƒ»œ p y š w.. x SiC (~50 µm, Zhengxing Abrasive C., Ltd, Dunhua, China), Silicn (~45 µm, 99% metals basis, Aldrich), Brn (amrphus pwder, 95/97%, HCST), Carbn (~45 nm, >99%, Krea Carbn Black C. Ltd., Inchn, Krea) w. w ƒ PEG (ply(ethylene glycl), (C H 4 O) n H O, Mn=400, 100, 4600) w. e ƒ yww š g w. yw SiC 1:4(wt%), g Ÿ (s v v ) ƒ ww. ƒƒ w Table 1 Table 1. Batch Cmpsitin f Prus SiC Ceramics sample SiC Cmpsitin (wt%) Si Carbn black B hllw micrsphere (additinal wt%) ùkü. yw 1 w š evapratr w g g. z x 10 MPa ƒw x w. ƒ m» w w»œx w, 3»œx 80 µm, ƒ 0.05 g/cm œx (hllw micrsphere, 09DET80, Expancel, Sundsvall, Sweden) w. œx t xk ply-methylmethacrylate.»œx ƒ ƒ yw k j š vl v (filter pressing) œ w r w. œ x ƒ z x w» w» w k vl v œ w. q p w š» ww, /w 5 C/min, 1300 C 3 wš, ƒƒ 1600, 1700, 1800 C 1~3 w. e w p y w» w, w r v e r w d wš, we w Prsimeter (AutPre IV Series, USA) w d w. q»œ SEM (JSM-5800, JEOL) w d w. m» p Capillary Flw Prmeter (CFP-100-AEL, PMI) w d w. œ SiC š 5 r span 30 mm e w 0.5 mm/min crss-head 3 š d w. 3. x š Si:C (ml rati) A B :1 C :1 D :1 E :1 F :1 G : Carbn w y w»œ x g m» 47«6y(010)

3 548 xá Á½w Á½ Á Fig. 1. Effect f carbn cntent n sintered density f prus SiC ceramics with variatin f sintering temperature. Fig.. Effect f carbn cntent n flexural strength f prus SiC ceramics with variatin f sintering temperature. ƒ š ky³ wš w ~50 µm j» ky³ w. w» ky³ œ y w SiC Si š e yww w»œ p y š w. w r w (B) % ƒw, w SiC r k»» p w j š14) š. p SiC w e» w 1500 C SiC t y w w. Fig. 1 e w y y d w. w w»œ SiC Si w m w 4%Ê46% wt% e w ¾ w ƒ, e w ƒw ƒ w w š. SiC (RBSC) œ e Si w e y w». ù ƒ mw e y j z ùküš. Fig. 3 š x w» p ùkü, 30~58MPa š. ù e w ƒw» p w w.» SiC (RBSC) œ e Si w SiC Si SiC x w» p w j w w w q. SiC œ SiC t e gq infiltratin w yœ, yww e SiC t Si t œ w z w z j w». ù 1700 C e (0. w%) 58 MPa w š. w ƒ ƒw ƒ ƒw ù, ƒ 1700 C ƒ» p w C w 1700 C» ƒ Si ƒ 1410 C š, 1670 C» 15) 1mmHg Siƒ w» w q. wr» p» w üy SiC w œ w, x ƒ w. p w SiC œ 43%»œ 3.9 MPa š 16), 50%»œ 10 MPa š 17). w g p w SiC 44%»œ 7.1 MPa š 18). Si w œ SiCƒ» œ w» p w. Fig. 3 e w y y ùk w wz

4 Si 결합 다공성 탄화규소의 미세구조 및 통기도 특성 - 카본 함량 변화 중심 549 공정을 통하여 카본을 혼합할 경우 카본이 SiC 분말의 표 면에 있지 않기 때문에 카본 함량의 증가는 결합강도를 증가시키기 보다는 치밀화를 억제하여 결합강도를 약화 시키는 역할을 할 수 있다. 이는 Fig. 의 실험결과와도 일치하는 경향을 보이고 있다. 그러나 Fig. 의 0. wt% 카본이 첨가된 1700 C 소결시편의 경우에는 곡강도 값의 증가 현상을 보이고 있다. 이는 미량의 카본은 SiC 표면 에 형성되는 SiO 를 환원 제거하는 등 긍정적인 효과를 보여 주기 때문으로 판단된다. 이는 기존의 반응소결 SiC 에서 카본의 주요 역할인 계면에 차 SiC 입자 형성을 통 한 강화에 비하여 차이점을 가진다. 즉 본 실험과 같이 단순 혼합공정인 경우, 충분한 양의 카본일 때 카본이 SiC 계면에서 주로 존재하지 않고, 액상의 Si 입자표면 또는 내부에서 차의 β-sic를 형성하게 되며, 이는 기계적 특 성 향상에 도움을 주지 못한다. 그러나 단순 혼합공정으 로 탄화규소 입자와 Si 입자를 습식 혼합하여 소결하는 경우에도, 미량의 제어된 카본(C)은 실제 새로운 차 βsic를 형성하기 보다는 Si 내부에 용해되거나 잔류된 상 태에서 아래의 반응식 에서와 같이 SiC 표면에 형성 되어 있는 산화피막인 SiO 를 환원 제거하기 위한 목적 으로 사용될 수 있다고 판단된다. 왜냐하면 산화피막인 SiO 는 SiC와 액상 Si과의 젖음성(wetting)을 저해하는 요 소로 작용하기 때문이다. 19,0) SiO +C = SiO(g)+CO (g) ; 050 K (1) SiO +3C = SiC+CO (g) ; 1800 K () Fig. 3. Typical fracture surfaces f prus SiC ceramics sintered at 1700C fr 3 h: (a) sample B (0. wt% carbn) and (b) sample F (1.01 wt% carbn). 낸 것이다. 카본 함량이 0. wt%인 Fig. 3(a)는 액상의 Si 이 SiC 입자를 잘 적셔서 결합을 증진시키는 역할을 한 것으로 판단된다. 그러나 카본의 함량이 1.01 wt% 첨가된 (b)의 경우에도 비교적 양호한 결합 모습을 보이고 있긴 하지만, 카본이 0. wt% 첨가된 (a)시편과 비교해서는 상 대적으로 액상 Si이 SiC 입자 사이에 네트워크를 공고히 하는 역할을 원활하게 수행하지 못하는 것으로 판단된다. 반응소결 공정은 고순도의 SiC와 카본 또는 카본으로 이루어진 성형체에 용융 Si을 침윤시키면 Si과 C이 반응 하여 형성된 새로운 SiC가 기존의 SiC와 Si 계면에 형성 되어 접합성을 증가시키는 공정 으로 알려져 있다. 그 러나 Si과 C의 반응으로 SiC가 형성되는 반응은 발열반 응으로 고순도 원료를 사용하지 않으면 계면에서 불순물 등의 가스가 발생됨으로 이에 대한 제어가 요구된다. 또 한 효율적인 반응소결 공정을 위해 탄화규소 표면에 카 본을 코팅하는 방법 등을 활용하여야만 효율적인 반응소 결 반응이 일어난다. 그러나 본 연구와 같은 단순 혼합 4-7) Fig. 4는 카본 함량 변화(a) 및 소결온도 변화(b)에 따른 통기도 변화를 나타내 것이다. Fig. 4(a)에 나타난 바와 같 이 카본 함량 변화에 따른 통기도 값은 압력차가 15 psi 에서 약 15 liter/min/cm 의 가스 유량을 보여 주었으며, 이 는 높은 통기도를 요구하는 진공척 또는 에어 베어링 등 에 적용이 가능한 수준을 보여준 것이다. 그러나 본 연구 의 실험변수인 카본 함량 변화에 따라 통기도의 큰 변화 는 보여 주지 못하였으나, 전반적으로 카본 함량이 증가 함에 따라 통기도는 조금씩 증가하는 경향을 보여 주었 다. 또한 소결온도가 증가함에 따라 통기도는 높아지는 경향을 보여 주었으나 1700 C와 1800 C에는 비교적 유사 한 통기도 값을 보여 주었다. Fig. 5는 카본이 첨가되지 않은 경우 시편 표면에 일부 과도한 액상이 형성된 것을 보여 주는 그림이다. 본 실험 에서는 액상으로 사용되는 Si의 양이 8.39~9.4 wt%로 충분히 많기 때문에 일부 바깥쪽으로 밀려 형성된 것이 다. 또한 용융 Si의 침윤양이 0% 이상 증가 시에는 일 부 작은 기공이 Si에 의해 폐쇄되는 현상을 관찰 할 수 있다. 또한 일반적인 반응소결 탄화규소인 경우에는 충분 한 카본 양으로 인하여 Si이 카본과 반응함으로 액상양이 제 47 권 제6호(010)

5 송인혁 박미정 김해두 김영욱 배지수 550 Fig. 6. 줄어들지만, 본 실험에서는 카본양이 작아서 소모되는 Si 이 거의 없기 때문에 과잉 Si이 형성된 것이다. 본 실험 에서는 충분한 액상 Si 조건에서 실험하기 위한 조건이었 으며, Si 양이 5 wt% 미만인 경우에는 이와 같이 과도한 액상 Si의 형상은 현저히 감소하였다. 기공 형성제 첨가 효과 본 연구에서는 높은 통기성을 가지면서도 기계적 강도 를 유지하기 위한 소재에 관한 연구에 초점을 맞추고 있 으며, 앞서 고찰된 조성에 대하여 기공도 및 통기도의 증 진을 위하여 중공형 미세구를 기공 형성제로 사용하여 미 세 구조 및 기공 특성을 분석하였다. Fig. 6에서 0.4 wt%의 중공형 미세구를 첨가한 경우 원 형으로 표시된 바와 같이 구형의 기공의 형성된 것을 관 찰 할 수 있었다. 이는 기공 형성제로 첨가한 중공형 미 세구의 크기인 80 µm와 거의 동일한 것을 관찰할 수 있 었다. 또한 중공형 미세구 0.4 wt%는 겉보기 부피 비율로 전체 분말의 겉보기 부피에 대하여 약 30 vl%에 해당하 는 부피로서, 기공도는 SiC의 이론 밀도와 Si 함량을 토 대로 계산한 결과 54.6%의 값을 보여주었다. Fig. 7은 중공형 미세구가 첨가된 경우와 첨가되지 않 은 경우를 비교하여 기공 특성을 수은 함침법으로 분석 한 결과이다. 기존의 중공형 미세구가 첨가되지 않은 경 우에는 개기공(pen pre)의 양이 33.5%에 기공 크기가 µm로 관찰되었으나, 중공형 미세구를 첨가한 경우 에는 개기공의 양이 44.9%에 기공크기가 3.04 µm에 이 르는 것을 관찰할 수 있었다. 이는 중공형 미세구의 첨가 를 통하여 기공도의 증가뿐만 아니라 평균 기공크기도 증 가되었다. 또한 중공형 미세구를 첨가한 시편의 기공도 계산치와 측정치가 차이가 나는 이유는 수은함침법에 의 해 측정된 결과가 개기공의 양만을 측정한 것으로서, 차 이 만큼인 9.7%가 액상 Si에 의해 형성된 폐기공(clse 3.. Fig. 4. Fig. 5. Air permeability changes f prus SiC ceramics: (a) effect f carbn cntent fr sintered bdy at 1700C fr 3 h, and (b) effect f sintering temperature at 0. wt% carbn cntent. The surface mrphlgy f specimen sintered at 1800C fr 1 h (sample A). 한국세라믹학회지 Micrstructure f the surface mrphlgy f sintered bdy fr sample G (0.4 wt% hllw micrsphere) at 1700C fr 3 h.

6 Si w œ ky³ m» p -e w y 551 ƒ 15 psi 40 liter/min/cm ƒ š.» y œ ƒ 15 psi 15~0 liter/min/cm š w ƒ m» ùkü. œx ƒ ƒ» p w, œx ƒ ƒ 58 MPa š w 1/ w w 8 MPa š ƒ. ù m» w» p sƒw. wz w w»œ x w y»œ j» m» ƒ w. 4. Fig. 7. Pre size distributin f prus SiC ceramics sintered at 1700 C fr 3 h: (a) Sample B (0 wt% hllw micrsphere) and (b) sample G (0.4 wt% hllw micrsphere).» ky³ œ y w SiC Si š e yww w šm» ƒ g w œ SiC w. w ~50 µm j» SiC g w, 1600~1800 C w. x mw œ,» p m» d 1700 C, e w 0. wt% ƒ w, š 58 MPa. e w ƒw» p w w, (0. wt%) e ƒ ƒ. m» p ƒ ƒw ƒw, e w w j y w. w»œ x œx ƒw m» ( 15 psi 40 liter/min/cm ƒ ) w w. Acknwledgment Fig. 8. Air permeability f prus SiC ceramics sintered at 1700 C fr 3 h: (a) Sample B (0 wt% hllw micrsphere) and (b) sample G (0.4 wt% hllw micrsphere). pre) q. Fig. 8 œx ƒ ƒ ƒ w m» w.» œx ƒ ƒ Fig. 3 ùk ù ƒ 15 psi 15 liter/min/cm ƒ ùkü ù, œx ƒ ƒ x» (The Center fr Advanced Materials Prcessing, CAMP) w,. REFERENCES 1. J. Saggi-Wyansky, C. E. Sctt, and W. P. Minnear, Prcessing f Prus Ceramics, Am. Ceram. Sc. Bull., 71 [11] (199).. P. Sepulveda, Gelcasting Fams fr Prus Ceramics, Am. Ceram. Sc. Bull., 76 [10] 61-5 (1997). 3. I. H. Sng, I. M. Kwn, H. D. Kim, and Y. W. Kim, Prcessing f Micrcellular Silicn Carbide Ceramics with a Duplex Pre Structure, J. Eur. Ceram. Sc., «6y(010)

7 55 xá Á½w Á½ Á (010) 4. H Osada, A Kani, S Katayama, T Kga, and K Ishizaki, Bending Strength and Electrical Resistivity f Prus Si- SiC Ceramics, Ceram. Trans., (199). 5. K. S. Se, S. W. Park, and H. B. Kwn, Fabricatin f Prus RBSC by Si Melt Infiltratin, J. Kr. Ceram. Sc., 37 [11] (000). 6. G. S. Ch, G. M. Kim, and S. W. Park, Fabricatin f Prus Reactin Bnded Silicn Carbide with Multi-Layered Pre Structure, J. Kr. Ceram. Sc., 46 [5] (009). 7. S. H. Yun, P. H. Tan, Y. D. Kim, and S. W. Park, Effects f Amunt f Carbn Surce and Infiltrated Si n the Prsity and Fracture Strength f Prus Reactin Bnded SiC, J. Kr. Ceram. Sc., 44 [7] (007). 8. F. J. Dias, M. Kampel, and H. Luhleich, Methd f Prducing Permeable, Prus Mlded Bdies f Silicn Carbide, US Patent (1985). 9. T. Tamamizu, K. Sat, T. Tanaka, and S. Sat, Sintered Silicn Carbide Prus Bdy Impregnated with Metallic Silicn, US Patent (1987). 10. A. K. Gupta, E. Gyarmati, H. Kreutz, R. Munzer, A. Naumidis, and H. Nickel, Methd f Making Prus Silicn Carbide Bdies, US Patent (1985). 11. C. R. Mrelck, Methd fr Making Shaped Silicn-Silicn Carbide Refractries, US. Patent (1983). 1. K. Y. Lim, Y. W. Kim, S. K. W, and I. S. Han, Effect f Carbn Surce n Prsity and Flexural Strength f Prus Self-Bnded Silicn Carbide Ceramics, J. Kr. Ceram. Sc., 45 [7] (008). 13. K. Y. Lim, Y. W. Kim, S. K. W, and I. S. Han, Effect f Aluminum Additin n Prsity and Flexural Strength f Prus Self-Bnded Silicn Carbide Ceramics, J. Kr. Ceram. Sc., 46 [5] 50-4 (009). 14. Y. W. Kim and J. G. Lee, Effect f Plycarbsilane Additin n Mechanical Prperties f Ht-pressed Silicn Carbide, J. Mater. Sci., 7 [17] (199). 15. J. F. Shackelfrd and W. Alexander, Ed, Thermdynamic and Kinetic Data, p. 30 in Materials Science and Engineering Handbk, third editin, CRC Press, USA, S. Ding, Y. P. Zeng, and D. Jiang, In-situ Reactin Bnding f Prus SiC Ceramics, Mater. Character, (008). 17. S. Ding, Y. P. Zeng, and D. Jiang, Thermal Shck Resistance f In-situ Reactin Bnded Prus Silicn Carbide Ceramics, Mater. Sci. Eng. A, (006). 18. S. Liu, Y. P. Zeng, and D. Jiang, Fabricatin and Characterizatin f Crdierite-bnded Prus SiC Ceramics, Ceram. Int (009). 19. G. W. Liu, M. L. Mul, F. Valenza, and A. Passerne, Survey n Wetting f SiC by Mlten Metals, Ceram. Int., (010). 0. K. S. Se, S. W. Park, and H. S. Sng, β-sic Frmatin Mechanisms in Si Melt-C-SiC System, J. Kr. Ceram. Sc., 36 [6] (1999). w wz

46.fm

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