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1 Jurnal f the Krean Ceramic Sciety Vl. 44, N. 5, pp. 279~283, Preparatin and Characterizatin f BCB Resin-BNT Cmpsite Substrate Materials Un-Yng Kim, Myung-Py Chun, Jung-H Ch, Byung-Ik Kim, Yng-Hyun Lee, Sung-Jae Myung, Ik-Hyun Han, and Dng-Uk Shin* Advanced Materials and Cmpnents Labratry, Krea Institute f Ceramic Engineering and Technlgy, Seul , Krea *Department Materials Science Engineering, Han-Yang University, Seul , krea (Received April 16, 2007; Accepted May 25, 2007) BCB Resin-BNT w»q p sƒ ½ Á tá yá½ Á xá Áw xá *», *w w œw ( ; ) ABSTRACT BCB Resin-BaNd 2 Ti 4 O 12 (BNT) cmpsites with BNT cntents were prepared by tape casting methd and epxy resin-bnt cmpsites were prepared by using heating press. Their dielectric prperties and micrstructures were investigated. The dielectric prperties such as dielectric cnstant and dielectric lss at 1 MHz fr epxy resin-bnt cmpsites and BCB resin-bnt cmpsites are imprved with an increase f BNT vlume fractin. The dielectric cnstant f the Epxy-BNT cmpsite increased frm 5.9 t 7.8 as the vlume fractin f BNT increased frm 15 t 25. The dielectric cnstant f the BCB-BNT cmpsite increased frm 9.1 t 15.5 as the vlume fractin f BNT increased frm 30 t 50. The dielectric behavir f BCB-BNT system can be explained by Lichtenecker s equatin. The dielectric cnstant f epxy resin-bnt cmpsite is smaller than that f BCB resin-bnt cmpsite. These results are cnsidered t be related with the dispersin f BNT filler in plymer matrix frm the result f SEM phtgraph. Key wrds : Plymer-ceramic cmpsite, Dielectric prperties, PCB 1. PCB(Printed Circuit Bard : z»q)» t» y w ql x k t k w»q»», { s, ful,, wœ» m»» w t., š d PCB,»» xy wy t( w, eq l)» q ü g j» š, ƒ û»q w š. wr, { s»» xy š qy»»q FR-4 w š, š q»q w v š. FR-4 jš, û. w w» w š Filler k -s w» Crrespnding authr : Dng-Uk Shin dwshin@hanyang.ac.kr Tel : Fax : w w»q w ƒ š. š q ZST(Zr 0.8 Sn 0.2 TiO 4 ) BNT š, s Resin s ƒ š ù, BCB Resin p. 1-6) š q»q w BNT- s BNT-BCB 2 -s»q w p w w. 2. x 2.1. Filler BNT(BaNd 2 Ti 4 O 12 ) BaCO 3 (, 99%), Nd 2 O 3 (KANTO, 99.9%), TiO 2 (š, 99.9%) w š w w w. yww» w k w 24 - w z, 80 C 24 w. q 1270 C( /w :5 C/min) 3 w w z q XRD(Max Science 279

2 김운용 전명표 조정호 김병익 이용현 명성재 한익현 신동욱 280 Fig. 1. Dielectric prperty cmparisn f BNT, BCB and epxy. KFX SE) 분석을 통해 합성됨을 확인하였다. BNT 의 소결 특성을 알아보기 위해 하소된 BNT 분말의 지름 을 약 10~12 mm, 두께 약 4~5 mm정도의 크기로 성형하 고, 1370 C(5 C/min)에서 3시간 유지하여 소결한 후 시편 의 특성분석을 Netwrk Analyzer(Agilent 8720ES, USA) 를 사용하여 유전 특성을 평가하였다. 폴리머로써 Epxy(TRANSOPTIC, buehler Ltd.)와 BCB (CYCLOTENE , Dw Chemical USA)를 사용하 였고 Fig. 1에 BCB, Epxy, BNT의 유전특성을 도식적으 로 나타내었다. BCB와 Epxy의 유전율은 각각 2.5와 3 그리고 Q값은 3000, 100이고, BNT는 유전율 90, Q값은 2000정도의 값을 가진다. 혼합방법 복합체 시편의 제조 분말 상태의 Epxy와 BNT를 유발을 사용하여 BNT의 함량에 따라 혼합을 하고 혼합한 파우더는 Munting Press (SIMPLIMET 3, buehler Ltd.)를 사용하여 다음과 같은 조 건으로 성형하였다. 성형조건으로는 160 C에서 700 psi로 10분간 유지하였 고, 지름이 약 25 mm, 두께가 약 2.8~3.8 mm인 샘플을 제작하였다. 특성 평가를 하기 위해 120 C에서 500 psi로 2분간 동판을 압착하여 전극을 형성하였다. 복합체 필름의 제조 액상의 BCB와 BNT 분말을 BNT 함량에 따라 Cnditining Mixer(ARE-250, Thinky USA)로 혼합하여 다음과 같은 혼합조건으로 페이스트를 만들었다. 혼합조건으로는 500 rpm 2분, 2000 rpm에서 5분간 혼합을 한 후 1000 rpm 에서 3분간 탈포를 실시하였다. 이렇게 만들어진 페이스 트를 Cu-Fil 위에 Hand Casting하고, 열처리하여 상부에 는 In/Ga 상온 전극을 도포하여 지름이 약 5 mm정도의 전극을 형성하였다. BNT/Epxy, BNT/BCB 이 두 가지 복합체 샘플은 LCR Fig. 2. XRD pattern f calcined BNT at 1270C. Meter(Agilent 4284A, USA)를 사용하여 정전 용량과 유전 손실을 측정하였다. 1 MHz에서 유전특성을 측정하고, 그 주파수에서 측정된 정전 용량으로 두 복합체의 유전율을 계산하였다. 그 미세구조는 광학 현미경(OLYMPUS BX51, Japan)과 SEM(SM-300, Tpcn)으로 관찰하였다. 3. 결과 및 고찰 선 회절 분석 3.1. X Fig. 2에서 보여주는 X선 회절 패턴은 1270 C에서 하소 된 BNT Pwder의 합성 정도를 잘 나타내어 주고 있다. JCPDS와 비교해 볼 때 BNT 피크가 잘 나타나고 있음을 알 수 있었고 BNT의 결정구조는 Lss가 적은 텅스텐 브 론즈 구조라는 것을 알 수 있다. Table 1과 Fig. 3에 텅스 텐 브론즈 구조와 하소된 BNT의 격자 상수를 나타내었 Table 1. Lattice Parameter f BNT JCPDS Experiment a 한국세라믹학회지 Fig. 3. Tungsten-brnze structure. b c

3 BCB Resin-BNT w»q p sƒ 281 Table 2. Dielectric Prperty f Sintered BNT Sample Frequency (GHz) Dielectric cnstant Quality factr Average Table 3. Dielectric Prperty f Epxy/BNT Cmpsite with BNT Cntents at 1 MHz Sample Thickness (mm) Diameter (mm) Capacitance Permittivity Lss (pf) BNT 15 vl% BNT 20 vl% BNT 25 vl% Table 4. Dielectric Prperty f BCB/BNT Cmpsite with BNT Cntents at 1 MHz Sample Thickness Diameter Capacitance Permittivity Lss (mm) (mm) (pf) BNT 30 vl% BNT 40 vl% BNT 50 vl% JCPDS w w w w ùkû p sƒ Table C w BNT r p Netwrk Analyzer d w t ùkü. š q p d Hakki-Cleman w p w. q ƒ 7) 4.5 GHz vjƒ ùkûš, vj vj w 91, Q Epxy-BNT Table 3 Epxy Matrix ü BNT Filler w k z p d wš» w. ƒ p ùký BNT w 25 vl% ƒ š 7, Lssƒ ùkû. Filler ƒ k ùkþ Filler ƒ g ƒ v w x. š Resin w Filler w w w w. 25 vl% Filler ƒ ƒ v x BCB-BNT Table 4 BCB ü BNT Filler jš LCR Meter d w l t ùkü. d Filler 50 vl% š 15.5, Lss Epxy ƒ Filler ƒw ƒw. w BNT Filler 50 vl% ƒ Epxy ƒ x w ƒ. Epxy BCB Resin w z x mw BCB-BNT Filler x mw Epxy- BNT w. w Lss» p w BCB-BNT ƒ Epxy- BNT w w. ƒ Resin w w š p ƒ Figs. 5, 6 ƒ Resin Filler ƒ j ƒ š. p Lss ƒ y ù. Resin p w Resin p» w j w x d w dwš x. Lichtenecker e 8,10) (Lgarithmic Rule). = + lgε t ν f lgε f ν r lgε r», ε t Filler Resin z š, ν f ν r Filler Resin v, ε f ε r Filler Resin ƒƒ ùkü. (1) w d BNT w Fig. 4 t w. (1) w Fig. 4. Cmparisn f expected data and experimental data f BCB-BNT cmpsite. (1) 44«5y(2007)

4 김운용 전명표 조정호 김병익 이용현 명성재 한익현 신동욱 282 험값은 BNT Filler 함량이 10~40 vl% 범위 내에서는 비 교적 잘 맞음을 보여준다. 한편, BNT 함량이 20 vl% 이 하, 그리고 50 vl% 이상에서는 이론값과 실험값과의 차 이가 증가하였다. 이러한 실험값과 이론값과의 차이는 BCB-BNT계 복합 체 내의 기공, 공극 등과 같은 결함에 의해서 발생된 것 으로 사료되며, 이들 결함은 열 처리시 유기용매의 휘발 에 의해 생성될 수 있다. Lichtenecker의 대수 법칙에는 이 러한 변수들을 포함하지 않았기 때문에 실제 실험값은 이 론값보다 작아졌다고 생각할 수 있다. 미세구조 Fig. 5는 Epxy/BNT 복합체의 분산 상태를 확인하기 위 하여 표면을 광학 현미경으로 관찰한 사진이다. 사진에서 도 관찰할 수 있듯이 Filler의 함량이 증가할수록 Resin의 양은 줄어들고 Filler의 양이 증가하는 것이 확연히 나타 났다. 또한 Filler들의 분산 상태는 상당히 안 좋은 것을 관찰하였고 Filler는 우선 Epxy와 잘 섞이지 않고 Epxy 주위에 조금씩 묻어 있었고, 분산 상태 또한 불규칙한 것 을 알 수 있었다. Fig. 5의 광학사진 관찰로 복합체의 미 세구조가 유전 특성에도 상당한 영향을 받는다는 것을 Table 3에서 확인할 수 있다. Fig. 6은 BCB 매트릭스 내 에 BNT를 함량에 따라 혼합하여 제작된 복합체의 단면 을 SEM으로 관찰한 사진이다. 사진에서 전체적으로 보 면 30 vl%에서 50 vl%로 증가하면서 Filler의 양이 늘어 나는 것을 확인할 수 있다. 반면에 Resin의 양이 확연히 줄어드는 것을 관찰할 수 있다. Epxy를 매트릭스로 한 복합체의 광학사진과 BCB를 사용한 복합체의 SEM사진을 비교하여 볼 때 BCB 복합 9) 3.4. Fig. 6. SEM images f BCB/BNT cmpsite fracture surface with BNT cntents (a)30 vl%, (b)40 vl%, and (c)50 vl%. 체에서 분산이 더 잘 되어 있음을 관찰하였다. 하지만 사 진에서 보다시피 Epxy의 경우보다 분산이 잘 되었다고 보지만 간혹 입자끼리 뭉쳐있는 것으로 볼 때 완전한 분 산을 이루었다고 판단하기는 힘든 것으로 사료된다. 지금 까지의 관찰 결과를 미루어 보아 복합체의 분산성은 그 유전특성에 상당한 영향을 미치는 것을 알 수 있다. 따라서 BCB 액상 Resin을 이용하여 후막성형으로 복합 체를 제조하는 것이 Epxy Resin을 이용한 일축성형에 비 하여 분산성을 좋게 하는 방법이라 생각된다. 4. 고주파용 기판재료로써 폴리머/세라믹 복합체는 세라믹 우수한 고주파 특성으로 인하여 상당히 주목받고 있는 연구 분야이다. 폴리머로 Epxy와 BCB를 사용하였 고, 세라믹으로 BNT를 사용하여 복합체를 제작하고 폴리 머에 따른 특성 변화를 조사하였다. BNT의 함량이 증가할수록, 유전특성은 향상되었으며, 임계치 이상으로 Filler의 함량이 증가되면, 바인더 역할 의 Resin 부족으로 인하여 성형등의 가공 문제가 발생하 였다. Epxy-BNT계에 비하여 BCB-BNT계가 좋은 Filler 의 함량을 보였으며, 유전율 및 손실등의 전기적 특성에 있어서도 BCB-BNT계가 우수하였다. Epxy 적용 시 BNT 함량이 약 25 vl%일 경우 그 유전 율은 7.8, Lss는 0.006의 값을 얻었다. 반면에 BCB 적용 시 50 vl%에서 유전율 15.5, Lss는 0.001의 값을 얻었다. 이러한 결과로 보면 Epxy를 사용 하였을 때 보다 BCB 를 사용하였을 때 유전율은 수배이상 차이가 나는 것을 확인하였다. 그 이유는 BCB 매트릭스에 Filler의 분산이 Filler의 Fig. 5. Optical images f epxy/bnt cmpsite surface with BNT cntents (a)15 vl%, (b)20 vl%, and (c)25 vl%. 한국세라믹학회지 결 론

5 BCB Resin-BNT w»q p sƒ 283 Epxy» w. w Resin BCBƒ Filler. s / w ƒ j p w j j w w š w. w s / w ƒ š q»q ww ƒ y w š, w w PCB j w w. REFERENCES 1. A. Silva, F. Azugh, R. Freer, and C. Leach, Micrwave Dielectric Ceramics in the System BaO-Li 2 O-Nd 2 O 3 -TiO 2, J. Eur. Ceram. Sc., (2000). 2. C.-H. Lu and Y.-H. Huang, Densificatin and Dielectric Prperties f Barium Nedymium Titanium Oxide Ceramics, Mater. Sci. Eng., B (2003). 3. A. Iachim, M. I. Tacsan, M. G. Banciu, L. Nedelcu, H. Alexandru, C. Berbecaru, D. Ghetu, and G. Stica, BNT Ceramics Synthesis and Characterizatin, Mater. Sci. Eng., B (2004). 4. H. Kbayashi and Y. Hskawa, Dielectric Cnstant Characteristics f a New Cmpsite Dielectric Material, J. Am. Ceram. Sc., 73 [6] (1990). 5. L. Ramaj, M. Rebred, and M. Castr, Dielectric Respnse and Relaxatin Phenmena in Cmpsites f Epxy Resin with BaTi 3 Particles, Cmpsite: Part A (2005). 6. D.-H. Ku, C.-C. Chang, T.-Y. Su, W.-K. Wang, and B.-Y. Lin, Dielectric Prperties f Three Ceramic/Epxy Cmpsites, Mater. Chem. Phys., (2004). 7. B. W. Hakki and P. D. Cleman, A Dielectric Resnatr Methd f Measuring Inductive Capacities in the Millimeter Range, PGMTT, December 24, (1959). 8. D.-H. Yn, J. Zhang, and B. I. Lee, Dielectric Cnstant and Mixing Mdel f BaTiO 3 Cmpsite Thick Films, Mater. Rearch Bulletin., (2003). 9. S.-D. Ch, S.-Y. Lee, J.-G. Hyun, and K.-W. Paik, Cmparisn Experimental Values and Theretical Predictins f the Dielectric Cnstant f Epxy/BaTiO 3 Cmpsite Embedded Capacitr Films, J. Micrelectrnics & Packaging. Sc., (2004). 10. A. V. Gncharenk, V. Z. Lzvski, and E. F. Venger, Lichtenecker s Equatin: Applicability and Limitatins, Optics Cmmunicatin (2000). 44«5y(2007)

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