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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 2, pp. 175~180, Effects f Glass Frit Size n the Sintering Behavir f Cu Terminatin Paste in MLCC Kyuha Lee, Byungjun Jen, Chang-Hn Kim, Yunggeun Kwn, Myungjun Park,G HyunHee Gu, Jiwn Uhm, Yung-Tae Kim, and Kang-Hen Hur* LCR Material Develpment Grup, Samsung Electr-Mechanics, Suwn , Krea *LCR Develpment Team, Samsung Electr-Mechanics, Suwn , Krea (Received Nvember 14, 2008; Revised December 13, 2008; Accepted December 22, 2008) Glass Frit ƒ MLCC Paste e w ³w Á Á½ zá«á Á x Á Á½ káx x*» LCR *» LCR q ( ; ; ) ABSTRACT Multilayer ceramic capacitrs (MLCCs) have cntinually been made smaller in size and larger in capacity in resent years. Hwever, the end terminatin electrde is still thick in many MLCCs. In this study, we used small grain glass frit t embdy thin film and highly densificatin in the end terminatin by imprve sintering driving frce with well-dispersin and rising surface energy. Pastes were fabricated using size changed glass frit, such as 0.1 µm, 0.5 µm, 1.0 µm, 4.0 µm. Fabricated pastes were applied 05A475KQ5 chip and fired varius sintering temperatures t analyze sintering behavir f pastes. Cnsequently, small glass frit used pastes have many merits than larger, such as well-dispersin, imprve crnercverage and surface rughness, pssibility f lw temperature sintering. Hwever, we cnfirmed that small glass frit used pastes have narrw sintering windw by rapid cmpletin f sintering densificatin. KeyG wrds : MLCCs, Terminatin electrde, Glass frit, Paste, Glass firt size, Sintering, Dispersin, Sintering windw 1. t t d eq l (Multilayer Ceramic Capacitr, MLCC)ƒ xy, š y mw w ùƒ» w eq l ü dy» dy rs» w š. 1) š 0603 ( mm 2 ) 1 µf MLCCù 1005 ( mm 2 ) 10 µf MLCC t 10 µm ü Ì e w š. ù» œ œ dy w e w» dy e y ƒ k œ v wš, xw r p d y w» ƒ v w. 2-7) r p w Crrespnding authr : Kyuha Lee kh6762.lee@samsung.cm Tel : Fax : ù Glass Frit y w r p š t ƒ w z w e w w w. 8-9) 2. x Glass Frit j» w w» w s³ 0.1, 0.5, 1.0, 4.0 µm w z w r p w. r p w 05A475 (1005, X5R, 4.7 µf) e sw z Prfile e þ k z» p sƒ mw Glass Frit j»» w Glass frit w Glass Frit Si-B-Zn-Ba-Ca-O 620 C y ùkü. Glass Frit» e w z 1200 C š k z þ k 175

2 이규하 전병준 김창훈 권영근 박명준 구현희 엄지원 김영태 허강헌 176 Prcess Cnditins fr Glass Frit Fabricatin Ntatin (D50 f glass frit) 4.0 µm 1.0 µm 0.5 µm 0.1 µm Table 1. Cmpsitins f Cu Pastes Paste N. 1.0 µm Cu 0.3 µm Cntent Glass frit 8.0% (/Cu, wt%) Cntent Dispersant (/Cu, wt%) Cntent Resin (/Cu, wt%) Slvent Prcess 24 h) 24 h) Attritin milling (3 mm 12 h) 24 h) Attritin milling (3 mm 17 h) 24h) RF plasma treatment (Ar 100 slpm, O2 50 slpm) Table 2. Table 3. Analysis f Glass Frits P1 P2 P3 P4 8.0% (D50:1.0 µm) 8.0% (D50:4.0 µm) 8.0% (D50:0.1 µm) (D50:0.5 µm) 0.1 µm(plasma) 0.5 µm(attritin) 1 µm(attritin) 4 µm(ball) D10 = 30 nm D50 = 70 nm D90 = 125 µm m2/g D10 = µm D50 = µm D90 = µm m2/g D10 = µm D50 = µm D90 = µm m2/g D10 = µm D50 = µm D90 = µm 1.45 m2/g SEM Size BET 로써 Flake 형태로 제조하고, 이를 다시 분쇄하는 공정을 거 쳐 원하는 입도로 조절한다. 본 연구에서는 평균입경 (D50) 이 0.1, 0.5, 1.0, 4.0 µm이 되도록 Glass Frit Flake를 분쇄하 였는데, 평균입경 4 µm 품은 건식분쇄 (ball milling)로 제조 하였다. 1 µm와 0.5 µm 품은 건식분쇄품을 다시 습식분쇄 (attritin milling) 함으로써 제조하였고, 0.1 µm 품은 건식분 쇄품을 플라즈마 열처리 함으로써 제조하였다. 각각의 Glass Frit 입도 별 공정조건을 Table 1에 나타내었다. 페이스트 제조 및 평가 제조된 각각의 glass frit을 적용하여 페이스트를 제조하 였다 (Table 2). Cu 분말은 1.0 µm와 0.3 µm 급 구형분말을 7 :3의 비율로 혼합하였고, glass frit과 분산제, 수지는 Cu 대비 8.0, 0.5, 9.0 wt%로 각각 조절하였다. 페이스트 원재 2.2. 한국세라믹학회지 료를 칭량한 후 선 혼합 후 3-Rll Mill (Inue, S7X16)을 이용하여 분산시켰으며 제조된 페이스트의 점도(Brkfield, HBDV-II+), 표면조도(Ksaka,ET4000A), 건조 후 막밀도 등 을 평가 후 05A475KQ5 기종에 간이 도포기(Fit,자체제작) 를 이용하여 도포하였다. 도포 조건은 Dipping 작업 시 175 µm, Bltting시 0 µm의 Paste를 깔고 작업을 진행하였다 Glass firt 분석 실험 결과 및 고찰 Table 3은 각각의 제법에 의하여 제조한 Glass Frit의 SEM (Tescan,VegaⅡLSM), 입도 (Hriba,LA-910), BET (Muntech,1208) 결과를 나타낸다. Plasma 제법 Glass Frit 의 경우 작은 입자 Size에 의한 표면에너지 증대로 인하여

3 Glass Frit ƒ MLCC Paste e w 177 Fig. 1. Viscsity (a) and Dry sheet Density (b) f Pastes. Fig. 2. Rughness Ra (a) and Rughness Rmax (b) f Pastes. Fig. 3. Capacitance f P3 and P4 Pastes with sintering temperature. x w» d ƒ w SEM mw ww. Glass Frit Sizeƒ t ƒw BET ƒw y w Paste Glass Frit w ƒƒ Paste w ƒ Paste Fig. 1. Paste Vehicle 45% š Glass Frit Cu t Well-Cating w Resin sw» Glass Frit Size Paste y ùkù. w Glass Frit Sizeƒ v ƒ ƒw» w w ùkü ù, 1.0 µm w Size j ƒ ù kù. w Paste» w d w Fig. 2. Glass Frit Sizeƒ y w. w Plasma Glass Frit Nan Size t ƒ w x w ƒ ƒ. 46«2y(2009)

4 이규하 전병준 김창훈 권영근 박명준 구현희 엄지원 김영태 허강헌 178. (a) Sectin Micrstructures f P3 and P4 Pastes with sintering temperature. (b) Surface Micrstructures f P3 and P4 Pastes with sintering temperature. Fig. 4 도포 칩 분석 각 Paste를 간이 도포기를 이용하여 05A475KQ5 기종에 도포하였으며 이 칩을 전극 소성 prfile 온도 별로 소성 중 칩을 급냉 시킨 후 용량 변화를 측정하였다. 미립의 Glass Frit을 사용시 용량이 구현되는 경향이 동일하였기 때문에 0.1 µm(p-4)와 4.0 µm(p-3) Glass Frit 사용 Paste의 용량 구 현 경향을 비교 Pltting하였으며 이는 Fig. 3과 같다. 0.1 µm(p-4)와 0.5 µm(p-1), 1.0 µm(p-2)의 미립 Glass Frit 를 사용하였을 경우 680 부터 초기 용량이 구현되기 시 작하여 720 C 이상의 온도부터 정상 용량대가 구현되었다. 이와는 다르게 4.0 µm Glass를 이용하여 제조한 Paste(P-3) 를 사용한 칩의 경우 720 부터 초기 용량이 구현되었으 며 770 부터 정상 용량대가 구현되었다. 미립의 Glass 사 용시 보다 초기 용량 구현 온도와 정상 용량 구현 온도가 상승하였음을 알 수 있다. 이와 같은 원인을 파악하기 위 3.3. 한국세라믹학회지 하여 각 칩 샘플들의 온도 별 미세구조를 분석하였다. 그 결 과 미립의 Glass Frit을 사용시 약 655 C 부근에서 Cu-Ni Ally의 생성이 가능하지만 4.0 µm Glass Frit을 사용시 700 부근에서부터 Cu-Ni Ally의 생성이 이루어지기 때문에 용 량 구현 경향성이 달라짐을 알 수 있었다. 측정한 각 칩 샘 플들의 온도 별 미세구조 분석 Data를 바탕으로 각 Paste들 의 온도 별 소결 거동을 정리하여 Table 4에 나타내었으며 이에 대한 단면과 표면 미세구조 사진은 Fig. 4와 같다. 용 량 구현과 마찬가지로 소결 거동 또한 미립의 Glass Frit(0.1, 0.5, 1.0 µm)를 사용시 동일한 소결 거동을 나타내 어 0.1 µm(p-4)와 4.0 µm(p-3) Glass frit 사용 Paste 소결 거동 분석 data만을 비교하였다. 미립의 Glass Frit을 사용한 P-1(0.5 µm), P-2(1.0 µm), P-4 (0.1 µm) Paste에서는 615 C에서부터 Cu 입자간의 Necking 이 생성되었으며 700 C부터 치밀화가 구현되었다. 이에 반

5 Glass Frit ƒ MLCC Paste e w 179 Table 4. Analysis f Pastes Sintering Behavir w j 4.0 µm Glass Frit w P-3 Paste 595æ l Cu Necking 755æ l e yƒ x. Glass frit Cu Necking ƒ Cu Paste Glass Frit Cu Bundary w Cu Necking ww Inhibitr w» q. Glass Frit w v ƒw» j Glass Frit w Cu š sw Cu Necking Inhibitr w z w. w Glass Frit e y x ƒ j Glass Frit w û j ƒ ù ƒw., w Paste Glass frit 0.1 µm~4.0 µm Size t w Glass Frit Ts(glass transitin temperature) j w e q. ƒƒ Glass Frit 615æ y» w 655æ x w Cu y w w. Glass Frit ù œ œ Vid û. Glass Frit Sizeƒ Vid j»ƒ e x ƒ w w., Glass Frit Sizeƒ Glass frit Paste ü š. Glass frit 655æ x w Cu y w w Cu š Wetting j. š Wetting Cu y ƒ w w š e y ƒ f w. w j Glass frit w» Glass Frit Wetting w. w Size Glass Frit j Size Glass Frit w ùkù Cu w û e y xw w. Glass Frit w Paste w û e x ƒ w y w. w Paste e ƒ x k ùe w Cu w ü»œ š Glass t ù y w. w Glass œ e w» Glass Frit y w» w v w q. 4. Glass Frit Sizeƒ MLCC Paste e w w x ww. Glass Frit Sizeƒ t Rughness w, š w e w, CrnerCverage z, ƒ q. w Glass Frit e yƒ» Windwƒ.» Glass Frit y w» w ƒ v w q. 46«2y(2009)

6 180 ³wÁ Á½ zá«á Á x Á Á½ káx x REFERENCE 1. Kishi, Y. Mizun and H. Chazn, Base-Metal Electrde- Multilayer Ceramic Capacitrs: Past, Present and Future Presectives, J. Appl. Phys., (2003). 2. Takahik Sakaue, Yshiaki Uwazumi, Takuya Sasaki and Taka Hayashi, Develpment f Cpper Pwder fr MLCC Electrde, CARTS., (2001). 3. Umesh Kumar, Cpper end Terminatin Develpment Methdlgy fr BME Based Capacitrs, CARTS., (2001). 4. Takahik Sakaue, Yasuhide TamaguchiS and Katsyhik Yshimaru, Study f Cpper Pwder Cmpsitin f the Paste fr Terminatin Electrde, CARTS., (2002). 5. Takahik Sakaue, and Katsyhik Yshimaru, Cpper Fine Pwder fr Terminatin Electrde in Mlcc, CARTS., (2003). 6. Jing zheng, jeff Schmersal, and Dave Lightweis, Enhancing Cpper Terminatin Technlgy fr MLCC s, CARTS., (2003). 7. Rudlf Huenert, Capacitr Grade Cpper Pwders, CARTS., (2003). 8. Gaskell, Resent Metal Thermdynamics ; Vl.1,G pp , Band Press, Seul, S.J. Kang, Sintering ; Vl.1, pp , Science Culture press, Seul, w wz

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