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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N., pp. ~9, 009. DOI: /KCERS Varius Filler Added CaO-Al -SiO Glass Cmpsites fr LTCC Substrate Applicatins Kwan S Kim, H Sn Jang, Hyunh Shin, In Tae Kim*, Shin Kim*, Yng Hyun Han*, 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 March 1, 009; Revised April 1, 009; Accepted April 0, 009) LTCC»q w w w CaO-Al -SiO w ½ Á y Á xyá½ k*á½ *Áw x*á w œw *( ) l (009 1 ; ; ) ABSTRACT Influences f ceramic filler types and dse n the sintering, phase evlutin, and dielectric prperties f ceramic/cao-al -SiO glass cmpsites were investigated. All f the specimens were sintered at 900 C fr h, which cnditins are required by the lwtemperature c-firing ceramic (LTCC) technlgy. Ceramic fillers f Al, SiO, kalin, and wllastnite were used. The additin f Al filler yielded the crystalline phases f alumina and wllastnite, and the densificatin ver 95% f the relative density was achieved up t 50 wt% additin f the filler. Fr the cases f the fillers f SiO, kalin, and wllastnite, crystalline phases f quartz, mullite, and wllastnite frmed, while the densificatin decreased mntnically with the filler additin. In verall, all the investigated fillers with 10 wt% additin resulted in a reasnable sintering (ver 95 %) and lw dielectric cnstants (less than 6), demnstrating the feasibility f the investigated cmpsites fr applicatin t a LTCC substrate material with a lw dielectric cnstant. Key wrds : CaO-Al -SiO, Filler, Ceramic/glass, LTCC, Lw dielectric cnstant 1. (Lw temerature C-fired Ceramics : LTCC)» qj w» q, p j q t w w. 1), LTCC» t xy w d» s d d dw w t xy» y. LTCC» w Ag(961 C) Cu(108 C) ƒ ƒ w, p q ceramic/glass w ƒ LTCC» q ƒÿ š. LTCC»q p., û ( y w ),, û (» Crrespnding authr : Sang Ok Yn Tel : Fax : y y),,., û q, œ q (0 ppm/ C). LTCC»q š Al 9.8, w ceramic/ glass w ƒ 7~8», y š y w û ƒ v w. w» y w. p LTCC»q lù š q(> 1 GHz)» š q z x û y w û, t ƒ š.,) CaO-Al -SiO (CAS ) q, yw w», w LTCC»q ceramic/glass w ƒ w. 4,5), Kumar 6) crdierite CAS ƒw anrthite (ε r =6) ceramic/glass w šw, Kim 7) CAS CaO-MgO-SiO (CMS ) Al yww w anrthite dipside

2 4 ½ Á y Á xyá½ ká½ Áw xá, (ε r =5.5) š š w. w Chi 8) Ch CAS Al, BaTi, CaTi, TiO, ZrO, MgO SiO w n w p šw.» CAS û silica-rich CAS w CAS w wš, w j q p e w w w š w. CaO-Al -SiO y yw kw p y š w. p kalin wllastnite Ÿ w LTCC»q ƒ mw.. x.1. CaO-Al -SiO x CaO-Al -SiO y yw. y Al (Kant, 99.0%) SiO (High Purity Chemicals, 99.9%) w. yw Al -SiO kalin CaO-SiO wllastnite kw, Ÿ w LTCC»q ƒ ƒ w mw» w, Ÿ w š m(kalin, Al :SiO ó45 : 55 wt%, û w ƒ ) ³z (wllastnite, CaO : SiO ó50 : 50 ml%, ) Ÿ w. w CaO-Al -SiO (CAS) w w, CaO, Al SiO y û» w B ƒw. 1, ƒƒ 9, 19, wt% e w s p» g yw w. yw ù ƒ 1500 C 0, k z þ g w. j mw 1 w š, ù» g k 4 mw w. z 100 C 4 w z 5 mesh m g CAS w... Ceramic/glass w» CAS ƒw LTCC»q ceramic/glass w w. CAS 10 ~ 50 wt% ƒ w s p» g k 4 w z 100 C 4 w. Ceramic/CAS glass w ƒƒ g e w 15 mm x š 50 MPa ƒ xw. x 10 C/min 900 C w z ¾ þw... p y p ³ wš dilatmeter(dil 40, Netzsch, Germany) w (Tg) y (Ts) d w. Ceramic/ glass w j r w j» e r (vernier calipers) w d z, w. pycnmeter (Accupyc 10, Micrmeritics, USA) w d w š, JCPDS card w. w ceramic/glass w Archimedes w d w. w w e y š wš d w ùkü, ƒ w (1) rule f mixture w. 9)», D w, W 1 w 1, W w, D 1 w 1, D w. W 1 + W D = W 1 D 1 + W D y w» w š X z»(d/max-500v/pc Rigaku, Japan) w 10 θ 80 Cu-Kα radiatin (40 kv, 50mA), 4deg/min d w. r FE-SEM(S-400, Hitachi, Japan) w w. j q p r sw q š Hakki-Cleman 10) w netwrk analyzer(hp870es, Agilent, USA) œ q f 0, œ q db œ s f œ q d w z, TE 011 mde œ vj w (ε r ) œ q t (Q f value) w.. š.1. CaO-Al -SiO p Fig. 1(a) CAS p d w Tg 740 C, Ts 841 C ùkü. w CaO-Al -SiO k y yw w, (1) w wz

3 LTCC»q w w w CaO-Al -SiO w 5 Table 1. Physical and Dielectric Prperties f the CAS Glasses CAS CAS-T10 CAS-TB CAS-T5 CaO Al SiO TiO B Density (g/cm ) Tg ( C) Dielectric cnstant Resnant frequency (GHz) Q f value (GHz) ,79,50 1,40,50 Remarks Current wrk Ref. 1 Fig. 1. (a) Dialtmetric curve (dl/l 0 ) f the CaO-Al -SiO - based (CAS) glass, (b) The investigated cmpsitins f CAS glass and CAS-T glass (ref. 1) in CaO-Al - SiO ternary diagram (in wt%) (B -, TiO -dping has nt been cnsidered). CAS Fig. 1(b) CaO-Al -SiO k Siƒ ew. w CAS w, L 11) Ca/Al/Si ƒ 1// kw y mw anrthite (CaAl Si O 8 ) kw, w TiO ƒw. Table 1 CAS L p w. CAS 900 C quenched-annealedw, L CAS-Tx 900 C w glass/ceramic. CAS ƒ, CAS CAS-TB ƒ w. ù CAS ƒ ƒ û ùkü, š anrthite(ε r =7) û ùkü. r,, CAS ƒ 900 C 8% û ùkü» e w ƒ x r ü w 1)»œ(ε r =1) w q., Shannn ƒ w v ü w ù ký, (dielectric plarizability) j f š š L w ƒ Tiƒ.9 Å 1,14)»., Appen Bresker ƒƒ y y ml% mw dw š šw. () w,» ε, ε i w» w ƒƒ y, P i ml%. ε ƒ w w, w w ƒ x w ù, j ƒ ƒw. 1 ε = ε i 100 P i CAS () mw w, Table CAS ƒ û w. () 46«y(009)

4 6 ½ Á y Á xyá½ ká½ Áw xá Table. Predicted Dielectric Cnstant f the CAS Glasses Via the Simple Rule f Mixture by Appen & Bresker s Equatin Cmpsitin Effective dielectric cnstant CAS CAS-T10 CAS-TB CAS-T5 wt%ml%wt%ml%wt%ml%wt%ml% CaO Al SiO TiO B Dielectric cnstant B ~8 p ƒ, w. TiO ƒ ƒ CAS anrthite» CAS û» ceramic/glass w ƒ ƒ w q... Ceramic/glass w p Ceramic/CAS glass w p š w» w, CAS CaO-Al -SiO ü w y (Al, SiO ) yw (Kalin, wllastnite) ƒƒ 10~50 wt% ƒw 900 C w. Fig. ceramic/cas glass w 900 C w, w (a) (b) y ùkü. w Al (JCPDS N :.98 g/cm ) SiO (JCPDS N :.65 g/cm ) JCPDS card w, kalin(.4 g/cm ), wllastnite(.09 g/cm ) CAS (.4 g/cm ) pycnmeter d w w. Al /CAS glass w w ƒw s w, w w p ùkü. CAS SiO ƒ 61 wt% Siƒ» SiO w ƒ (W K < S) w» q. p ceramic/cas glass w w ƒ CAS w j w» e y w w w w. w 15) ceramic/cas glass w ƒ Fig.. Change in (a) X-Y shrinkage and (b) relative density f the investigated ceramic/cas glass cmpsites as a functin f filler additin (wt%) sintered at 900 C (Al (A), SiO (S), kalin (K), and wllastnite (W)). 900 C, CAS y ƒ 841 C» w q. Fig. ceramic/cas glass w 900 w z, r w X- z d w. (a, b, c, d) (a', b' c', d') Al (A), SiO (S), kalin (K) wllastnite(w)ƒ ƒƒ 10, 50 wt% ƒ ceramic /glass w ùkü. Al /CAS glass w crundum(jcpds N ) wllastnite CaSi (JCPDS N ) x, CaSi () z (100 peak). SiO /CAS glass w quartz(jcpds N ) ƒ. Kalin/CAS glass w 10 wt% ƒw w wz

5 LTCC 기판재료 응용을 위한 다양한 충전제 함유 CaO-AlO-SiO 유리 복합체 연구 Fig.. 7 Pwder XRD patterns f the investigated ceramic/cas glass cmpsites as a functin f filler additin (wt%) sintered at 900C. 것으로 보아 kalin이 CAS계 유리에 완전히 녹아 들어가 비정질이 된 것으로 판단되며, 50 wt%를 첨가하였을 때에 는 mullite의 Al Si O (JCPDS N ) 결정상이 관 찰되었다. Wllastnite/CAS glass 복합체의 경우 CaSiO (JCPDS N ) 결정상만 관찰되며, unknwn 결정상 이 존재하는 것은 저급의 wllastnite 천연 광물에 포함된 불순물에 기인한 것으로 보인다. Kumar 등 은 CaO-Al O SiO 를 1:1: mle로 합성하여 1500 C에서 열처리할 경우 화학양론적(stichimetric) anrthite 결정상을 갖는 화합물 이 합성되지만, glass/ceramic 복합체의 경우에는 1:0.7:.9 mle로 혼합한 후 1400 C에서 용융 및 급냉시켜 제 조할 경우에만 anrthite 결정상이 생성된다고 보고하였다. 또한 Chi와 Ch 의 연구에서는 CaO-Al O -SiO -B O 유 리에 Al O 와 SiO 를 충전제로 사용하였을 때 Al O 의 경 우에는 Al O 의 주상과 anrthite의 차상이 관찰되지만, SiO 의 경우 SiO 의 주상만 관찰된다고 보고하였다. 따라 서 본 연구에 사용된 CAS계 유리는 SiO 함량이 많은 유 리 조성(1.01 :.1 : 6.85, wt%)이며, 유리의 연화 온도(Ts) 가 841 C로 높아 유리의 결정화 및 재분배 과정을 거치 기 어렵기 때문에 anrhite 결정상이 생성되지 않는 것으 로 판단된다. Fig. 4는 ceramic/cas glass 복합체를 900 C에서 소결한 시편의 내부 미세구조를 나타낸 것이며, 미세구조 사진의 조성 표기는 상기 Fig. 과 같다. 10 wt%의 세라믹 충전 제가 첨가된 모든 복합체는 치밀한 내부 구조를 갖지만, 50 wt% 첨가된 경우 상기 선수축율과 상대밀도의 결과와 같이 폐기공이 발생하여 소결 밀도가 저하되는 것을 알 수 있다. 더욱이 충전제 종류에 따라 상대밀도가 감소(A >K>W>S)하는 것과 같이 미세구조에서도 폐기공의 크 1 6) 8) Fig. 4. Micrstructure f the investigated ceramic/cas glass cmpsites as a functin f filler additin (wt%) sintered at 900C. 기와 수가 증가되는 것을 관찰할 수 있다. 이는 충전제의 함량이 증가함에 따라 CAS계 유리의 양은 감소하기 때 문에 액상소결을 위한 소결구동력이 감소되기 때문이며, 또한 CAS계 유리는 Si가 많은 조성이기 때문에 SiO 함 유가 많은 세라믹 충전제일수록 유리에 덜 용해되기 때 문에 시편 내부에 폐기공이 형성된 것으로 해석된다. 일 반적으로 ceramic/glass 복합체의 치밀화에 미치는 영향은 액상소결의 기공 채움(pre filling) 모델 과 ceramic/glass 복합체의 점성유동 소결이론 을 응용해서 설명이 가능 하다. 액상소결의 기공 채움 모델은 액상 소결이 시작되 면 액상이 생성되고, 먼저 액상은 시편 중심부로 모이고 (liquid cagulatin), 그 후 액상이 많이 몰린 비교적 치밀 한 부분이 넓어져서 액상이 시편 전체에 고르게 분포되 어 시편 전체가 고립 기공만을 포함한 비교적 균일한 조 직으로 되며(liquid redistributin), 고립 기공은 결국 액상 으로 채워져 소멸된다고 보고되었다(liquid filling pre). 또 한 ceramic/glass 복합체의 소결 기구에서, 초기 단계는 액 상유리의 재분배 과정으로 유리상이 원래의 자리로부터 세라믹 입자 사이의 모세관 형태의 기공 채널로 이동하 며, 고상 입자의 재배열 과정을 거쳐 유리에 둘러싸인 잔 여 기공들은 치밀화의 마지막 단계인 점성 유동을 통해 제거되어 치밀한 소결체를 얻을 수 있다고 보고되어 있 다. 따라서 최대 치밀화를 갖는 복합체를 제조하기 위해 16) 15) 제 46 권 제 호(009)

6 8 ½ Á y Á xyá½ ká½ Áw xá yw w w w. w ceramic/glass w 70 wt% ƒw, ƒw x w», y CAS p ceramic/glass w p j w e ƒw w... Ceramic/glass w p Fig. 5 ceramic/cas glass w 900 C w, w y ùkü. Bsman 17) Havinga Wiener w» œ sww d l w,»œ(ε r =1) w ƒ w š šw.» p w ƒw s»œ w ƒ w. ù ceramic/glass w ƒ 7 w û», š»œ w yƒ j., (Kalin, wllastnite)/cas glass w w ƒw ƒ w p ùkü, p 10 wt%ƒ ƒ Al /CAS glass w ) 4.8 û 19)ƒ ùkü kalin(ε r =5.1) wllastnite(ε r =5) Al û». SiO /CAS glass w SiO 0 wt% ƒ j q p d w ƒw. j q p d w netwrk analyzer d w TE 011 mde œ vj w w, œ vjƒ». ù 10 wt% ƒ Fig. 5. Change in dielectric cnstant f the investigated ceramic/cas glass cmpsites as a functin f filler additin (wt%) sintered at 900 C. Fig. 6. Change in quality factr f the investigated ceramic/ CAS glass cmpsites as a functin f filler additin (wt%) sintered at 900 C. ƒ, 4. û ùkü, SiO ƒ.8 û». Al /CAS glass w w ƒw ƒ s ƒw p ù kü. Al ƒ w yƒ j»,»œ w, w Al ƒ 9.8 CAS 5.54» w q. Fig. 6 ceramic/cas glass w 900 C w, w t y ùkü. (Al, wllastnite)/cas glass w y w ƒw t ƒw p ùkü, Al (0,000 GHz) 0) wllastnite(5,98 GHz) t ƒ CAS (1,800 GHz) x». ù t Al w Al /CAS glass w ƒ,000 GHz û t ùkü, w ü w w Al ƒ» w. j q œ q t w w w., št û g w.» ü (intrinsic lss) (extrinsic lss)., ü» ƒ j ü w y.,»,»œ, w, w. 1) SiO /CAS glass w» d d w wz

7 LTCC»q w w w CaO-Al -SiO w 9 ƒw š, w SiO kalin x ¾ t w ƒ š w t w y ³ w». ù kalin 10 wt% ƒw,600 GHz ƒ w t ùkü. 4. CaO-Al -SiO w j q p e w w w š w» w 10 ~ 50 wt% ƒw w. 10 wt% ƒw, 900 C ƒ w, p Al ƒw w p s w, SiO, kalin wllastnite w p ùkü. Al, SiO, kalin wllastnite 10 wt% ƒ ceramic/cas glass w 900 C w p š w, (ε r = 5.4, 4., 5.07, 4.8) œ q t (Q f value =,90, 1,790,,60,,10 GHz) ùkü. SiO /CAS glass w ƒ 4. ƒ û, w kalin wllastnite Ÿ w w j q p ùkü LTCC»q ƒ w q. Acknwledgment» wx mw. REFERENCES 1. Y. J. Chi, J. H. Park, J. H. Park, S. Nahm, and J. G. Park, Middle- and High-Permittivity Dielectric Cmpsitins fr Lw-Temperature C-fired Ceramics, J. Eur. Ceram. Sc., 7 [4] (007).. M. Kn, H. Takagi, T. Tatekawa, and H. Tamura, High Q Dielectric Resnatr Material with Lw Dielectric Cnstant fr Millimeter-Wave Applicatins, J. Eur. Ceram. Sc., 6 [10-11] (006).. Y. Imanaka, Multilayered Lw Temperature Cfired Ceramics (LTCC) Technlgy; pp. 1-17, Springer, Berlin, Y. Kbayashi and E. Kat, Lw Temperature Fabricatin f Anrthite Ceramics, J. Am. Ceram. Sc., 77 [] 8-4 (1994). 5. C. L. L, J. G. Duh, and B. S. Chiu, Lw Temperature Sintering and Crystallisatin Behaviur f Lw Lss Anrthite-Based Glass-Ceramics, J. Mater. Sci., (00). 6. C. J. Dileep Kumar, E. K. Sunny, N. Raghu, N. Venkataramani, and A. R. Kulkarni, Synthesis and Characterizatin f Crystallizable Anrthite-Based Glass fr a Lw- Temperature Cfired Ceramic Applicatin, J. Am. Ceram. Sc., 91 [] 65-5 (008). 7. J. H. Kim, S. J. Hwang, W. Y. Sung, and H. S. Kim, Effect f Anrthite and Dipside n Dielectric Prperties f Al / Glass Cmpsite Based n High Strength f LTCC Substrate, J. Mater. Sci., (008). 8. I. J. Chi and Y. S. Ch, Effects f Varius Oxide Fillers n Physical and Dielectric Prperties f Calcium Aluminbrsilicate-Based Dielectrics, J. Electrceram., (In Press). 9. T. Takada, S. F. Wang, S. Yshikawa, S. J. Jang, and R. E. Newnham, Effect f Glass Additins n BaO-TiO -W Micrwave Ceramics, J. Am. Ceram. Sc., 77 [7] (1994). 10. B. W. Hakki and P. D. Cleman, A Dielectric Resnatr Methd f Measuring Inductive Capacities in the Millimeter Range, IRE Trans. Micrwave Thery Tech., MTT (1960). 11. C. L. L, J. G. Duh, B. S. Chiu, and W. H. Lee, Lw-Temperature Sintering and Micrwave Dielectric Prperties f Anrthite-Based Glass-Ceramics, J. Am. Ceram. Sc., 85 [9] 0-5 (00). 1. R. D. Shannn, Dielectric Plarizabilities f Ins in Oxides and Flurides, J. Appl. Phys., 7 [1] (199). 1. H. Schlze, Glass:Nature, Structure and Prperties; pp.18, Springer, New Yrk, A. A. Appen, Versuch zur Klassfizierung vn Kmpnenten Nach Ihrem Einflub auf die Oberflachenspannung vn Silikatschmelzen, Silikattechnik, (1954). 15. R. M. German, Liquid Phase Sintering, Plenum Press, New Yrk, W. D. Kingery, Implicatins f Sintering Theries with Regard t Prcess Cntrls, Tras. VIIth Inter. Ceram. Cng., (1960). 17. A. J. Bsman and E. E. Havinga, Temperature Dependence f Dielectric Cnstants f Cubic Inic Cmpunds, Phys. Rev., 19 [4] (196). 18. D. A. Rbinsn, Measurement f the Slid Dielectric Permittivity f Clay Minerals and Granular Samples Using a Time Dmain Reflectmetry Immersin Methd, Sil Sci. Sc. Am. J., (004). 19. W. Cai, T. Jiang, X.Q. Tan, Q. Wei, and Y. Li, Develpment f Lw Dielectric Cnstant Calcium Silicate Fired at Lw Temperature, Electrn. Cmp. Mater., (00). 0. H. Wang, Q. Zhang, H. Yang, and H. Sun, Synthesis and Micrwave Dielectric Prperties f CaSi Nanpwder by the Sl-Gel Prcess, Ceram. Inter., (008). 1. W. D. Kingery, H. K. Bwen, and D. R. Uhlmann, Intrductin t Ceramic; Vl., pp. 05-6, Jhn Wiley & Sns, New Yrk, «y(009)

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