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1 Journal of the Korean Ceramic Society Vol. 44, No. 2, pp. 98~102, Effect of Recycling Time on Stability of Colloidal Silica Slurry and Removal Rate in Silicon Wafer Polishing Eun-Suck Choi and So-Ik Bae R&D Center, Siltron Inc., Gumi , Korea (Received November 14, 2006; Accepted December 28, 2006) Recycling g e Á p» ( ; ) ABSTRACT The stability of slurry and removal rate during recycling of colloidal silica slurry was evaluated in silicon wafer polishing. The particle size distribution, ph, and zeta potential were measured to investigate the stability of colloidal silica. Large particles appeared as recycling time increased while average size of slurry did not change. Large particles were identified by EDS (energy dispersive spectrometer) as foreign substances from pad or abraded silicon flakes during polishing. As the recycling time increased, ph of slurry decreased and removal rate of silicon reduced but zeta potential decreased inversely. Hence, it could be mentioned that decrease of removal rate is related to consumption of OH ions during recycling. Attention should be given to the control of ph of slurry during polishing. Key words : Recycling, Slurry, Abrasive, ph, Zeta potential, Removal rate 1. g r( w g r) j œ(ingot) (slicing) s (polishing) mw. s CMP(chemical mechanical polishing) yw» y w wš w skyw ù w. g r skyw» w 1-3) w, g e(colloid silica) ƒ e f. CMP œ» w, ƒ e f yw w r wš sky w, e e z 4-6) ph, y, ƒ w œ š,» z q r t w ü sw q œ w œ. g r s œ j 1 s 2 s. 1 s œ ƒœ d sky w œ š, 2 Corresponding author : So-Ik Bae Tel : Fax : s r sky e» g yw œ. 2 s r t w s w 1z w. 1 s œ š w g r t w e recyclingw w. g r w recycling w z w y ü g e w, w yw w. yw g e w w w š, g r w. g r 1 s m w, s recycling w s, ph, k (zeta potential) sƒw š, recycling ph y wafer w š w. 2. x g eƒ y g r Nalco 2371 (Rohm and Haas Co.) w 1 s 98

2 Recycling g e 99 Fig. 1. Schematic diagram of slurry recycling process for silicon wafer polishing. recycling w w r w š w. x 28 wt% g e w w, g r s w g e w 2.5 wt% yww w. Recycling 500 r y w» w 250 recycling mw z 50% wš, j w ù 250 recycling w r ww. Fig. 1 g r recycling w ù kü. œ kj ƒ œ š r w œ kj z œ w. Recycling w» w œ kj vl mw r œ w. ph(handylab ph/lf12, Schott), k (ELS 8000, Otsuka Electronics), x (scanning electron microscopy, ERAX-8000) EDS(energy dispersive spectrometer, Voyager3000) w sƒw. ph y y 200 mm g r(p-type, (100)) polishing machine(poli-500, GNP Tech.) mw ww z z Ì d (ADE 9500, ADE Corp.) mw y w. g r w w Table 1 ùkü. Table 1. Experimental Parameters of Polishing Used in This Study Slurry Commercial Nalco 2371 colloid silica Pad Suba 640 Flow rate 700 ml/min Pressure 260 g/cm 2 Wafer size 200 mm, P-type silicon wafer ph 9~12 Fig. 2. Average abrasive size with recycling time. 3. š Fig. 2 recycling ELS 8000 m w w g e s³ j» y ù kü v. Recycling w s ³ j» ƒ ù s ƒ. r w ph w y wš e f w w. 7,8) r g e ƒ e f,. wš e f ü g e ³ w jš yw w r w w. w yw w g e w ³ w š j» ƒw. w 9) 1 s ww recyclingw s³ j» yƒ recycling w yw š y w. recycling ELS 8000 w w light scattering intensity distribution Fig. 3 ùk ü. Recycling (Fig. 3(a)) s wù ³ s š. 100 (Fig. 3(b))¾ recycling z wù ³ s. w 180 (Fig. 3(c)) z s wù ³ s s(ot) š š, Fig. 3(d) 470 recycling s š. w. g r q š r yw» w ƒ w. r, q recycling š, w g 44«2y(2007)

3 최은석 배소익 100 Fig. 3. Fig. 4. Size distribution of slurry with various recycling time by light scattering intensity at (a) 0, (b) 100, (c) 180, and (d) 470 min. Scanning electron microscope images of slurry with the recycling time at (a) 0 min, (b) 470 min, and (c) sludge deposited after 470 min recycling time. 카 입자 안정성이 일부 저하가 예상이 된다. 유입된 불순 물 중 마모된 패드는 콜로이드 실리카 입자와 결합하여 거대 입자를 형성하거나 자체가 거대 입자로써 존재하게 된다. 연마 입자 외에 슬러리 내부에 존재하는 거대 입자의 존 재를 확인하고자 좀더 상세한 분석을 진행하였다. Fig. 4 는 recycling 과정 전후와, recycling 후 슬러리 침전물의 주사 전자현미경 사진이다. 슬러리의 침전물을 분석하기 위해서 미세 그리드에 액상의 슬러리를 떨어뜨려 건조한 후에 진행하였다. Recycling 전 슬러리는 Fig. 4(a)의 사진 처럼 약 90 nm 크기의 구형 콜로이드 실리카 연마 입자 들이 잘 분포되어 있음을 알 수 있다. 하지만 Fig. 4(b)의 470분 recycling 한 후 슬러리의 경우 콜로이드 실리카 외 에 이물질( 표)이 포함되어 있음을 확인할 수 있다. Fig. 4(c)는 470분 recycling된 슬러리를 채취하여 2~3시간 정 도 방치 후의 침전물 형상이다. 이를 보면, 이전의 형상 과는 다르게 구형의 연마 입자는 이물질과 혼재되어 그 형상을 파악하기가 힘들다. 이들은 대부분 연마 과정 중 한국세라믹학회지 Fig. 5. Energy dispersive spectra of the sludge deposited after 470 min recycling time. 에 발생한 부산물로써 실리콘 미립자 및 패드 성분으로 예측된다. Fig. 5는 Fig. 4(c)의 침전물의 성분을 EDS 분석을 통해 분석한 결과이다. 침전물은 C, O, Si 성분 외에는 검출되 지 않았다. 이들의 근원을 살펴보면 Si와 O는 슬러리의 연마 입자인 콜로이드 실리카와 연마된 실리콘 웨이퍼에 기인한 것이다. 실험에 사용된 패드는 주 성분이 폴리에 스테르 및 폴리우레탄 계열로써 C, H, O 등의 원소로 구 성되어 있어 C의 경로는 패드임을 알 수 있다. 결국 연 마 부산물로써 검출된 이물질이 슬러리의 연마 입자, 연 마된 실리콘 웨이퍼와 연마된 패드에 의해서 발생된 것 임을 확인할 수 있었다. Fig. 6은 슬러리 recycling이 진행되는 동안 슬러리의 제 타 전위와 ph 변화를 나타낸 그래프이다. ph의 경우 recycling 시간이 지남에 따라 점점 감소하고 있음을 확인 할 수 있다. Recycling 시간 280분에서 ph가 증가한 것 10)

4 Recycling g e 101 Fig. 6. Zeta potential and ph with the recycling time of slurry. x w 250 recycling z 50% wš œ w». z recycling û ph w. ph w z r z y e f ƒ û, ü w OH g r t Si ww Si-OH xk ey OH». w ph Si w w»z r w w. k y ph y. k y w w w. m g e ph y ph 4.5 ( k ƒ 0 ) š k. g e w š š» w ü š g x k. k ƒ w g y. ƒ wš w» w ph ƒ w. recycling w ph g r w w ph y j z r Ì d mw sƒw. Fig. 7 ph y ùkü v. r» ph 10.6 û ph HCl ƒw, KOH ƒw w. Fig. 6 w ph y ü OH y w. OH g r t Si w yd(hydroxide layer, Si-OH) x Fig. 7. The change of removal rates as a function of ph of slurry. š, ü w ù 8) x w ƒ. phƒ û OH w j w. ph t e y 2 yd(sio 3 ) x ƒ w x. 8) Fig. 7 ph y y mw 10.6 ph 0.61 µm/min. recyclingw r w, g e wš, g r y w» w ph w w. 4. g e g r CMP w s recycling r w š w. Recycling s³ j» w. w light scattering intensity distribution w s r 100 recycling w w sƒ ùkûš, EDS l q g g e y w. Recycling ƒw ph w, k ƒw w ùkü. ph ü OH. g r OH Si yw w g e» w w, g r t Si ww OH v r 44«2y(2007)

5 102 Á j wù w. recyclingw w, ph ü g e r w w w w w. REFERENCES 1. R. K. Singh and R. Bajaj, Advances in Chemical Mechanical Planarization, Mater. Res. Soc. Bull., 27 [10] (2002). 2. A. C. West, H. Deligianni, and P. C. Andricacos, Electrochemical Planarization of Interconnect Metallization, IBM J. Res. & Dev., 49 [1] (2005). 3. S. B. Yeruva, C. W. Park, and B. M. Moudgil, Modeling of Polishing Regimes in Chemical Mechanical Polishing, Mater. Res. Soc. Symp. Proc., 867 W (2005). 4. G. B. Basim and B. M. Moudgil, Slurry Design for Chemical Mechanical Polishing, KONA, (2003). 5. B. J. Palla and D. O. Shah, Stabilization of High Ionic Strength Slurries Using the Synergistic Effects of a Mixed Surfactant System, J. Colloid Interface Sci., (2000). 6. B. J. Palla and D. O. Shah, Stabilization of High Ionic Strength Slurries Using Surfactant Mixtures: Molecular Factors That Determine Optimal Stability, J. Colloid Interface Sci., (2002). 7. V. E. Gaishun, O. I. Tulenkova, I. M. Melnichenko, S. A. Baryshnin, Y. A. Potapenok, A. P. Xlebokazov, and W. Strek, Preparation and Properties of Colloidal Nanosize Silica Dioxide for Polishing of Monocrystalline Silicon Wafers, Mater. Sci., 20 [2] (2002). 8. D. Graf, A. Schnegg, R. Schmolke, M. Subren, H. A. Gerber, and P. Wagner, Morphology and Chemical Composition of Polished Silicon Wafer Surfaces, Electrochem. Soc. Pro., (1996). 9. H. G. Kang, T. Katoh, J. G. Park, U. Paik, and H. S. Park, Influences of ph and Concentration of Surfactant on the Electrokinetic Behavior of a Nano-Ceria Slurry in Shallow Trench Isolation Chemical Mechanical Polishing, J. Kor. Phys. Soc., 47 [4] (2005). 10. J. H. So, S. H. Bae, S. M. Yang, and D. H. Kim, Preparation of Silica for Wafer Polishing via Controlled Growth of Commercial Silica Seeds, Kor. J. Chem. Eng., 18 [4] (2001). w wz

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