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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 6, pp.g609~614, 009. DOI: /KCERS Prperties f Lw Temperature Sintered Prus Ceramics frm Alumina-Zinc Brsilicate Glass Kwan S Kim, Ki Yung Sng, Sang Yeup Park, Shin Kim*, Sung Jin Kim, and Sang Ok Yn Department f Ceramic Engineering, Kangnung-wnju Natinal University, Gangneung 10-70, Krea *Cermtech C., Ltd, Gangnung Science & Industry Park, Gangneung 10-40, Krea (Received June 8, 009; Revised July 0, 009; Accepted August, 009) ù- ³ w œ p ½ Á» Á Á½ *Á½ Á w œw *( ) l ( ; ; ) ABSTRACT The lw-temperature preparatin f prus ceramics was carried ut using mixtures f alumina-zinc brsilicate (ZBS) glass. The cmpsitins f alumina-zbs glass mixture with PMMA pre-frmer were unfrtunately densified. Because PMMA was evaprated belw the sftening pint f ZBS glass (588 C), the densificatin thrugh the pre-filling caused by the capillary frce might ccur. Hwerver, thse with carbn pssessed pres where carbn was evaprated abve the sftening pint. The prus ceramic having 5% prsity was successively fabricated by the lw-temperature sintering prcess belw 900 C using 45 vl% f alumina, 45 vl% ZBS f glass, and 10 vl% f carbn as starting materials. KeyG wrds : Prus ceramics, Al O, Zinc brsilicate glass, Pre frmer, Lw temperature sintering 1. œ (prus ceramics) 15~95% ƒ»œ» e w ƒ w p ƒ š y w w,»œ,»œ»œj» s w. p œ ù š w w ü, ü, ü y ü w ƒ š. œ w, û ü w, ƒ vl,, k, w š, üy» w»œ»œ j» w» œx w ƒ y š. 1,) œ, š Crrespnding authr : Sang Ok Yn syn@kangnung.ac.kr Tel : Fax : s, s,»œ. -7)»œj»ƒ 0.1~60 µm š,»œ 40% w p w, ƒ, š s (reticulated structure) xk w, ywš ü š s wew w z k, w w. s, w, y, t sw ü s yw z xp ü wš, w w s k z w w»œ»œ w w.» œ j» ƒ j»œ w x ù l v x»œ yw w š. w wƒ ƒ w x š»œ w œ» ü x»œ ƒ x,»œ j»»œ,»œ sƒ»œ ƒ w š w. w»œ 609

2 610 ½ Á» Á Á½ Á½ Á w w j» w»œ ƒw œ w.»œ {»œ w»œ p w w., œ w š w w œ w, p - œ.» š œ ƒ w ceramic-glass w» w 900 C w ƒ w œ w wš w. w, œ w ƒw,»œx w œ w e w š wš w.. x.1. ³ ù(α-al O, Kant, 99.5%, 5 µm),»œx PMMA(Plymethyl methacrylate, Pcera, 99.0%, 10 µm) carbn( š yw, 99.7%, 5 µm) w. w ³ (zinc brsilicate glass, ZBS glass) glass w w. š yw(99.9%) ZnO, B O SiO, ƒ ƒ 65, 5 10 wt% e w s p» g yw w. yw ù ƒ 1500 C 0, k z þ(quenching) g ZBS glass w. ZBS glass j (disk mill) mw 1 w š, ù» g k 4 (ball mill) mw w. z 100 C 4 w z 5 mesh m g ZBS glass(5 µm) w. w» ZBS glass p w» w (windw glass, W) q, m w 5 µm w w š, XRF(X-Ray Flurescence Spectrmeter, Rigaku, Japan) w w Na O(1.%), MgO(4.5%), SiO (69.%)»k (1%)ƒ w - e... Ceramic-glass w œ Al O -glass w Table 1,, w š w» w Al O 45 vl% glass(windw glass ZBS glass), 10 vl%»œx (carbn) ƒw Table 1. Specimen Ntatin f Sample with Additin f Carbn and PMMA Cmpsitin (vl%) w w.,»œx w w š w» w Al O vl% ZBS glass, 10 0 vl%»œx (carbn PMMA) ƒw w w. œ Al O - glass w 15 mm mx w, 50 MPa ƒ w xw,»œx PMMA carbn» { j» w ƒƒ 50 C 700 C ƒƒ 1 (burn ut) e z, 10 C/min 700~900 C œ» w... y p ³ wš Dilatmeter(DIL 40, Netzsch, Germany) w (Tg) y (Ts) d w.»œx { š STA(Simultaneus Thermal Analyzer, Netzsch, Germany) w y y w. Al O -ZBS glass w j r e r (vernier calipers) w d z, w. Al O JCPDS card(n ) w,»œx pycnmeter (Accupyc 10, Micrmeritics, USA) w d w. Al O -glass w Archimedes w d w, ƒ w (1) rule f mixture w, 8) D Al O (A) Windw glass (W) V 1 + V + V = V 1 D 1 V D V D ZBS glass (Z) Carbn (C) PMMA (P) 50A-50Z A-45W-10C A-45Z-10C A-40Z-0C A-45Z-10P A-40Z-0P D w, V 1 w 1 v, V w v, V w v, D 1 w 1, D w, D w. Al O -glass w»œ () mw w, (1) w wz

3 ù- ³ w œ p 611 Fig. 1. Thermgravimetric analysis f the pre frmer, PMMA and carbn. P ( %) 1 D b = 100 D th P w»œ (prsity), D b w (bulk density), D th w () (thery density). w, w»œ j» w» w Prsimeter(AutPre IV 9510, Micrmeritics, USA) w. y w» w š X z»(d/max-500 V/PC Rigaku, Japan) w 10 θ 80 Cu-Kα radiatin (40 kv, 50 ma), 4 deg/min d w. r FE-SEM(S-400, Hitachi, Japan) w w.. š.1.»œx p ZBS glass Ts( y ) 588 C, windw glass Ts 750 C, Fig. 1»œx PMMA carbn (thermgravimetric) w.»œx w p (5~1000 C) d w, PMMA 80 C z wƒ 450 C { ( 0%), carbn 60 C {» w 1000 C( 45%)¾ w., carbn { w, d y v w w ù, d œ s CO ƒ y». Fig.. Changes in (a) linear shrinkage and (b) prsity f Al O -ZBS glass cmpsite and Al O -glass cmpsites with carbn as a functin f sintering temperature: (Al O (A), ZBS glass (Z), windw glass (W), and carbn (C))... œ Al O -glass w p Fig. Al O -ZBS glass w carbn ƒ Al O -glass w (a) y (b)»œ y ùkü.»œx ƒw Al O -ZBS glass w Al O ZBS glass ƒƒ 50 vl% ƒ (50A-50Z), carbn ƒ Al O -glass w Al O (A) glass(z, W)ƒ ƒ ƒ 45 vl%, carbn(c) 10 vl% ƒ (45A-45Z-10C 45A-45W-10C). 50A-50Z 45A-45Z-10C w 700~900 C¾ ƒ ƒw»œ yƒ, 45A-45Z-10C w 46«6y(009)

4 61 ½ Á» Á Á½ Á½ Á Fig.. Pwder XRD patterns f Al O -ZBS glass cmpsite and Al O -glass cmpsites with carbn sintered at 900 C: ((a) 50A-50Z, (b) 45A-45Z-10C, and (c) 40A- 40W-10C). 50A-50Z w û (7.5%)» œ (s³ 5%) ùkü. ù 45A-45W-10C w 0%»œ ùkü, ƒ ƒw ƒ»œ s w w ùkü. 45A-45W- 10C w w ƒ k œ w 900 C w œ w» ww q, w ƒ ƒ v w. Fig. 50A-50Z w carbn ƒ 45A-45Z- 10C 45A-45W-10C w 900 C w z, w X- z. 50A-50Z w 45A- 45Z-10C w ZnAl O 4 (JCPDS N ) Al O (JCPDS N ), Al 4 B O 9 (JCPDS N ) Zn B O 6 (JCPDS N )., 45A-45W-10C w Al O NaAlSi O 4 (JCPDS N ) x, peak intensityƒ x û w...»œx w œ Al O -ZBS glass w p Fig. 4 50A-50Z w»œx (carbn, PMMA) ƒ ƒ Al O -ZBS glass w (a) y (b)»œ y ùkü.» œx ƒ ƒ Al O -ZBS glass w Al O (A) ZBS glass(z) ƒƒ vl%, carbn(c) PMMA(P) ƒƒ 10 0 vl% ƒ (45A-45Z-10C, 40A-40Z-0C, 45A-45Z-10P 40A-40Z-0P)., 0 vl% Fig. 4. Changes in (a) linear shrinkage and (b) prsity f Al O -ZBS glass cmpsite and Al O -ZBS glass cmpsites with pre frmer as a functin f sintering temperature. carbn ƒ w Archimedes w»œ d r q.»œx w 700~900 C¾ ƒ ƒw»œ yƒ. ù 50A-50Z w carbn ƒ w û, PMMAƒ ƒ w û»œ ùkü, PMMA w ƒw p ƒw ùkü. ceramic-glass w 9)» w wz

5 알루미나-아연붕규산염 유리를 이용한 저온 소결 다공성 세라믹스의 제조 및 특성 Fig Pwder XRD patterns f AlO-ZBS glass cmpsites with pre frmer sintered at 900C: (a) 45A-45Z-10C, (b) 45A-45Z-10P, and (c) 40A-40Z-0P. 래의 자리로부터 세라믹 입자 사이의 모세관 형태의 기 공 채널로 이동하며, 중기의 고상 입자의 재배열 과정을 거친 후, 마지막 단계인 점성 유동을 통해 유리에 둘러싸 인 잔여 기공들이 제거되면서 치밀화된다. 더욱이 세라믹 에 액상 전구체를 침투, 열분해 및 고상반응 과정을 통한 치밀화 기술, 즉, 공기와 같은 기체를 함유하고 있는 다공체 내 액상을 침투하는 메커니즘은 압축된 기체의 내 부 반대압력이 모세관 압력과 똑같아 질 때 다공체 내부 로 액상이 유입되면서 치밀화 일어나는 것으로, 본 연구 에서도 이와 유사한 소결 특성을 잘 나타내고 있다. 따라 서 PMMA가 휘발되면서 시편 내에 인위적인 기공을 형 성하여 액상이 유동할 수 있는 부피가 증가되며, ZBS glass 연화 후 유리 액상이 모세관 압력에 의해 기공 채 움 현상이 일어나 치밀화가 이루어지게 되는 것으로 판 단된다. 더욱이 PMMA 함량이 증가함에 따라 치밀화되 는 것은 비록 Al O 입자에 대한 ZBS glass의 유효 액상 량은 한정되어 있지만, PMMA 휘발 함량의 증가에 따라 시편 내에 다량의 기공이 형성되어 모세관압력이 액상 내 부의 압력보다 더 커지기 때문으로 판단된다. Fig. 5는 45A-45Z-10C, 45A-45Z-10P 및 40A-40Z-0P 복합체를 900 C에서 소결한 후, 분쇄한 분말 X-선 회절 분석 결과이다. 기공형성제 종류 및 함량에 관계없이 Fig. (a)의 50A-50Z 복합체와 같은 결정상이 생성되었으며, 이 는 기공형성제가 Al O -ZBS glass 복합체의 결정화에 영 향을 주지 않는 것을 알 수 있다. Fig. 6은 50A-50Z, 45A-45Z-10P 및 45A-45Z-10C 복합 체를 900 C에서 소결한 소결체의 시편 내부를 FE-SEM으 로 관찰한 결과이다. (c)의 45A-45Z-10C 복합체는 상기 -절에서 설명한 것과 같이 ZBS glass가 연화된 후 10,11) Fig. 6. Micrstructure f AlO-ZBS glass cmpsite and AlO-ZBS glass cmpsites with pre frmer sintered at 900C: (a) 50A-50Z, (b) 45A-45Z-10P, and (c) 45A45Z-10C. carbn의 휘발되기 때문에 다공성 세라믹스가 제조된 것 을 관찰할 수 있다. 반면 (b)의 45A-45Z-10P 복합체의 경 우 소량의 폐기공이 존재하지만, 상기 소결 특성에서 설 명한 것과 같이 (a) 50A-50Z 복합체보다 더 치밀화된 것 을 관찰할 수 있다. 따라서 PMMA가 첨가된 Al O -ZBS glass 복합체는 PMMA 휘발(80 C) ZBS glass 연화 (588 C) 를 거쳐 소결이 이루어질 것이며, carbn이 첨가 된 경우에는 ZBS glass 연화(588 C) carbn의 휘발 (60 C) 따라 진행되며, 즉, Al O -ZBS glass 복합체에서 치밀화(densificatin)와 다공화(prus)는 기공형성제의 휘 발 온도 및 ZBS glass 연화 온도에 의존하는 것으로 판 단된다. 4. 결 론 Ceramic-glass 복합체 제조 기술을 응용하여 900 C 이하 의 저온에서 소결이 가능한 다공성 복합체를 제조하기 위 해, 유리 종류, 기공형성제의 종류 및 함량이 저온 소결 제 46 권 제 6호(009)

6 614 ½ Á» Á Á½ Á½ Á œ w e w š w.»œx ƒw Al O -ZBS glass w 900 C w,»œx w ZnAl O 4 Al O, Al 4 B O 9 Zn B O 6 x j, Al O -ZBS glass w PMMA ƒw e y, carbn ƒ œyƒ ƒw p ùkü.»œx { ZBS glass y, œ Al O -ZBS glass w w» w y z»œx ƒ { w. Al O -ZBS glass w 10 vl% carbn ƒw w, 700 C l w»œ ùkü, 900 C w 5%»œ œ Al O -ZBS glass w w. REFERENCES 1. J. G. Kim, H. C. Shin, J. H. Shim, W. S. Ch, and J. H. Oh, Develpment f High-Perfrmance Prus Ceramic Membrane, Ceramist, 4 [6] (001).. R. W. Rice, Prsity f Ceramics; pp , Marcel Dekker, Inc., New Yrk, P. Sepulveda, Gelcasting Fams fr Prus Ceramics, Bull. Am. Ceram. Sc., 76 [10] 61-6 (1997). 4. D. J. Green, Fabricatin and Mechanical Prperties f Spheres, J. Am. Ceram. Sc., 68 [7] (1985). 5. T. Fujiu, G. L. Messing, and W. Huebner, Prcessing and Prperties f Celluar Silica Synthesized by Faming Slgel, J. Am. Ceram. Sc., 7 [1] (1990). 6. Y. J. Kim and O. J, Bae, Fabricatin f Prus Clay Ceramics Using Surfactant, J. Kr. Ass. Crys. Grwth, 1 [1] (00). 7. S. J. Lee and H. D. Kim, Fabricatin f Prus Al O Ceramics Using Thermplastic Plymer, J. Kr. Ceram. Sc., 41 [7] (004). 8. T. Takada, S. F. Wang, S. Yshikawa, S. J. Jang, and R. E. Newnham, Effect f Glass Additins n BaO-TiO -WO Micrwave Ceramics, J. Am. Ceram. Sc., 77 [7] (1994). 9. D. Dunstan and L. R. White, A Capillary Pressure Methd fr Measurement f Cntact Angle in Pwders and Prus Media, J. Cllid and Interface Sci., 11 [1] 60-4 (1986). 10. O. Sudre and F. F. Lange, Effect f Inclusins n Densificatin; Micrstructural Develpment in an Al O Matrix Cntaining a High Vlume Fractin f ZrO Inclusins, J. Am. Ceram. Sc., 75 [] (199). 11. F. A. Dullien, Prus Media-Fluid Transprt and Pre Structure; p. 157, Academic Press, New Yrk, w wz

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