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1 Journal of the Korean Ceramic Society Vol. 46, No. 6, pp. 673~678, DOI: /KCERS Effect of MgO Buffer Layer on the Structural Properties of Sputter-grown ZnO Thin Film Young Soo Lim Green Ceramics Division, Korea Institute of Ceramic Engineering and Technology, Seoul , Korea (Received August 25, 2009; Revised August 31, 2009; Accepted September 1, 2009) rl y w y d z w» ( ; ; ) ABSTRACT The effect of MgO buffer layer on the structural properties of sputter-grown ZnO thin film was investigated. Sapphire (0001) and Si (100) substrate were used for the growth and MgO buffer layer was inserted between ZnO thin film and the substrate. X-ray diffraction pattern indicated that enhanced crystallinity in the ZnO thin film grown was achieved by inserting very thin MgO buffer layer, regardless of the substrate type. The strain in the ZnO thin film could also be controlled by the insertion of the MgO buffer layer, and tendency of the strain was strongly dependent on the substrate type. Key words : ZnO, MgO, Buffer layer, Sputtering 1., Ÿ e, ƒ l»», Ÿm š» e š, w Ÿ ƒš. y Mg, Cd, Be sw y y (ZnxM1- xo,» M = Mg, Cd, Be) q Ÿw x ˆ(direct band gap) ƒ,» š y 2» (exciton binding energy) w { xw. w û 1,2) œ w ƒ ƒ w, Ÿ ƒ w. 3), Ÿn ƒ» n, n p l. 4,5) w p ƒ y w w w» w w y v. w y Corresponding author : Young Soo Lim yslim@kicet.re.kr Tel : Fax : (molecular beam epitaxy), r (pulsed laser deposition), yw» (chemical vapor deposition), rl x ¾ ù, rl y ƒ w x ¾ ƒ w. 6-8) ù, wš rl»q w w»,» ƒ. rl w y, q (0001)»q y d d(buffer layer) w y g.»q 10 nm y d w, w 40%¾ w y. 2. x g (100)»q q (0001)»q RF v p rl w, y rl k z, r 673

2 임영수 674 터링법에 의해 산화아연 박막을 증착시켰다. 이 때 스퍼 터링 챔버의 기본압력(base pressure)은 Torr 이하 이며, 스퍼터링 시 증착압력(working pressure)은 9 mtorr 로 설정하였다. 스퍼터링 가스로는 아르곤과 산소가 1:3 으로 혼합된 가스를 이용하였다. 산화마그네슘 완충층은 400 C의 실리콘 및 사파이어 기판 위에 60 W의 출력으로 각각 200, 400, 800 및 1600초 동안 형성되었으며, 이러 한 완충층 위에 동일한 가스, 온도 및 압력에서 산화아연 박막을 100 W의 출력으로 7200초간 증착하였다. 이상과 같이 증착된 산화아연 박막의 단면과 평면을 Hitachi S4800 주사전자현미경(scanning electron microscope, SEM) 으로 15 kv의 가속전압에서 분석을 수행하였으며, 산화마 그네슘 완충층이 이루는 계면은 Tecnai사의 G2 F30 STwin 투과전자현미경(transmission electron microscope, TEM)으로 300 kv의 가속전압으로 분석하였다. 산화아연 박막의 결정성과 변형량 분석은 Bruker사의 D4 Endeavor x-선 회절분석기(x-ray diffractometer, XRD)를 이용하여 40 kv와 40 ma의 조건에서 Cu Kα 선을 이용하여 분석 을 수행하였으며, 조성분석은 VG ESCALAB 250 x-선 광 전자 분광분석기(x-ray photoelectron spectroscopy, XPS)에 서 Al Kα 선을 이용하여 수행하였다. 6 o 3. 결과 및 고찰 Fig. 1의 (a)는 산화마그네슘 완충층 없이 사파이어 기 판 위에 증착된 산화아연 박막의 단면 주사전자현미경 상 을 보여준다. 그리고, Fig. 1의 (b)~(e)는 산화마그네슘 완 충층을 각각 200, 400, 800 및 1600초간 증착한 후, 그 위 에 증착된 산화아연 박막의 단면을 보여주며, 이때 산화 마그네슘 완충층의 두께는 10 nm 이하로 너무 얇기 때문 에 주사전자현미경 상에서는 구분이 되지 않는다. 완충층 의 증착시간이 800초인 경우까지는 100 W의 출력에서 7200초간 증착된 산화아연이 150 nm의 두께를 가지는 평 탄한 박막으로 증착된 것을 확인할 수 있다. 그러나, 완충 층의 증착시간이 1600초인 경우에는 파단면에서 산화아 연 박막이 주상성장(columnar growth)을 한 형상이 관찰되 었으며 또한 표면에 50 nm 내외의 요철이 존재하는 것이 확인된다. 이러한 경향은 평면 주사현미경 상인 Fig. 1의 (f)~(j)에서도 관찰되는데, 완충층의 증착시간인 800초인 경우까지는 완충층이 증착되지 않은 경우와 큰 차이가 관 찰되지 않으나, 1600초간 완충층을 형성한 경우에는 주상 성장에서 기인한 육각형의 요철구조가 관찰된다. 상기와 같이 제작된 산화아연 박막의 결정성을 x-선 회 절기를 이용하여 분석을 수행하였으며, 이때 얻어진 산화 아연 (0002) 피크의 반치폭(full width at half maximum, FWHM)을 Fig. 2(a)에 나타내었다. 완충층의 증착시간이 0초인 것은 완충층을 형성하지 않고 사파이어 기판위에 한국세라믹학회지 Fig. 1. SEM micrographs of ZnO thin film grown on sapphire (0001) substrate. (a)~(e) are cross-sectional and (f)~(j) are plan-view micrographs. (a) and (f): no MgO buffer layer, (b) and (g): MgO deposited for 200 sec, (c) and (h): MgO deposited for 400 sec, (d) and (i): MgO deposited for 800 sec, (e) and (j): MgO deposited for 1600 sec. 바로 산화아연 박막을 증착한 것을 의미한다. Fig. 2(a)에 서 완충층의 증착시간이 800초 까지는 박막의 반치폭이 지속적으로 감소하여, 완충층이 없는 경우에 비해 최대 40%의 바치폭 감소가 나타났다. 이는 스퍼터링법을 이용 한 산화아연 박막의 증착 시, 산화마그네슘 완충층이 그 위에 성장되는 산화아연 박막의 결정성을 증진시킨다는 것을 의미한다. 그러나, 완충층을 1600초간 형성시킨 경 우에는 다시 산화아연 박막의 결정성이 나빠지는 현상이 관찰된다.

3 rl y w y d z 675 Fig. 2. (a) 2-theta position of (0002) XRD peak of ZnO thin film grown on sapphire (0001) substrate and (b) corresponding FWHM as a function of the deposition time of MgO buffer layer. Fig. 2(b) q»q y (0002) vj 2θ ùkü, d 800 ¾ y š, z w w. Bragg equation z ƒ ƒ f w, s w w y c- w ƒ ƒw ùkü. y d y x w ƒ. Fig. 3(a) Fig. 2 x- z» ƒ w, 800 k y d w y n x. 60 W 800, y 3nm ƒ Ì, y <0002> w w ùkù. y d y w, y Fig. 3. (a) A high-resolution TEM micrograph of the ZnO/ MgO/sapphire interface and (b) corresponding XPS depth profile (MgO deposition time = 800 sec). d w w w l» w. ù, w w g» (epitaxial relation), y w y w. TEM l, ¾ y gƒ y d Ì 1nm 6nm ƒ w. 800 k d y w» w x- Ÿ Ÿ» w ¾ w ww, Fig. 3(b) ùkü. y t Zn w w,»q Al 46«6y(2009)

4 임영수 676 Fig. 5. Fig. 4. SEM micrographs of ZnO thin film grown on silicon (100) substrate. (a)~(e) are cross-sectional and (f)~(j) are plan-view micrographs. (a) and (f): no MgO buffer layer, (b) and (g): MgO deposited for 200 sec, (c) and (h): MgO deposited for 400 sec, (d) and (i): MgO deposited for 800 sec, (e) and (j): MgO deposited for 1600 sec. 의 함량이 감소한다. 이때 계면에서 Mg의 함량이 최대가 되며, 이로부터 산화마그네슘 완충층이 산화아연 박막과 사파이어 기판 사이에 잘 형성되어 있음을 확인할 수 있다. 산화마그네슘 완충층의 효과는 사파이어 기판 뿐만 아 니라 격자의 정합성이 없는 실리콘 (100) 기판을 사용하 였을 때에서도 관찰되었다. Fig. 4(a)와 (f)는 산화마그네 슘 완충층이 없이 실리콘 (100) 기판 위에 성장된 산화아 연 박막의 단면 및 평면 주사전자현미경 상을 보여주며, (b)~(e)와 (g)~(j)는 산화마그네슘 완충층을 각각 200, 400, 한국세라믹학회지 (a) 2-theta position of (0002) XRD peak of ZnO thin film grown on silicon (100) substrate and (b) corresponding FWHM as a function of the deposition time of MgO buffer layer. 800 및 1600초간 성장시킨 후 그 위에 증착된 산화아연 박 막의 단면 및 평면을 보여준다. 100 W에서 7200초간 실리 콘 (100) 기판 위에 증착된 산화아연은 완충층의 유무에 관계없이 모두 주상성장을 하였으며, 이는 단면 주사 전자 현미경 상에서 관찰되는 세로방향의 결 무늬로부터 확인 할 수 있다. 산화마그네슘 완충층의 성장시간이 800초까 지는 완충층이 없는 경우와 같이 그 두께가 220 nm이지만, 완충층의 두께가 1600초에 이르면 그 두께는 약 180 nm이 며 표면에 요철구조가 형성되는 것을 확인할 수 있다. 평 면 주사전자현미경 상인 (f)~(j) 역시 이와 유사한 경향성 을 보여준다. 완충층의 증착시간이 200 및 400초인 경우 에는 완충층이 존재하지 않은 경우와 유사한 표면 형상 이 관찰되지만, 800초간 완충층을 형성하였을 경우에는 표면에 50 nm 가량의 폭을 가지는 요철구조가 형성된다. 그리고 1600초간 완충층을 형성한 경우에는, 표면에 육각 형의 요철구조가 관찰되며 이는 단면 주사전자현미경 결 과와 일치한다.

5 rl y w y d z 677 g (100)»q y x- z» w ww, y (0002) vj es Fig. 5(a) ùkü. Fig. 5(a) d 400 ü x w ù, d 800, y d Ì ƒ 3nm 11%. w g (100)»q d 1600 z, y w»q. Fig. 5(b) g (100)»q y (0002) peak 2θ ùkü, d 800 ¾ y, 1600 d x w w w., q»q ƒ g»q y d w y k y x w ƒ. y d w y w q»q w w. y 9-12) rocksalt ƒ, q»q d Stranski-Kristanov(S-K)» w. w 10) S-K» w y q»q (island growth) w, w ƒ y d y lateral growth w œw y. w y z 11,12) Å y q»q w w w w, Fig. 2» w. 10) ù, q»q w g (100)»q w. Fig. 5(a), y d g es ƒw 800 z 11% ƒ. w ƒ q»q» l y d y j, g»q w w»» y y ww». ù, y d w z, Fig. 4 x y w w. l, y d w y z»q y g» w zw, w y d rl w y x w y w. 4. y d rl y e w w w. q (0001) g (100)»q y d wš y w,»q w y 40%¾ x- z mw ³ w. w q (0001)»q w y d 800 k ¾ y ƒ 1600 w w, g (100)»q 800 ¾ ƒ 1600 w y. rl w y, y d y j z x w w ³ w. Acknowledgment»» (No ) w. REFERENCES 1. Y. Igasaki and H. Saito, Substrate Temperature Dependence of Electrical Properties of ZnO:Al Epitaxial Films on Sapphire (1-210), J. Appl. Phys., (1991). 2. M. H. Whang, S. Mao, H. Feick, H. Q. Yan, Y. Y. Wu, H. Kind, E. Weber, R. Russo, and P. D. Yang, Room-temperature Ultraviolet Nanowire Nanolasers, Science, (2001). 3. D.-K. Lee, S. J. Lee, J. Bang, and H. Yang, Wet Chemical Etching of Transparent Conducting Ga-Doped ZnO Thin Films by Oxalic and Formic Acid, J. Electrochem. Soc., 156 D211-D14 (2009). 4. Y. B. Kim, J. U. Kim, D. K. Choi, J. M. Hong, and I. D. Kim, Electrically Stable Low Voltage Operating ZnO Thin Film Transistors with Low Leakage Current Ni-doped Ba0.6Sr0.4TiO 3 Gate Insulator, J. Electroceramics, (2009). 46«6y(2009)

6 S. Kim, J. Seo, H. W. Jang, J. Bang, W. Lee, T. Lee, and J.- M. Myoung, Effects of H 2 Ambient Annealing in Fully 002-textured ZnO:Ga Thin Films Grown on Glass Substrates Using RF Magnetron Co-sputter Deposition, Appl. Surf. Sci., (2009). 6. A. Ohtomo, M. Kawasaki, Y. Sakurai, Y. Yoshida, H. Koinuma, D. Yu, Z. K. Tang, G. K. L. Wang, and Y. Segawa, Mater. Room Temperature Ultraviolet Laser Emission from ZnO Nanocrystal Thin Films Grown by Laser MBE, Sci. Eng. B, (1998). 7. F. K. Shan, G. X. Liu, W. J. Lee, and B. C. Shin, The Role of Oxygen Vacancies in Epitaxial-deposited ZnO Thin Films, J. Appl. Phys., (2007). 8. S. Bethke, H. Pan, and B. W. Wessels, Luminescence of Heteroepitaxial Zinc Oxide, Appl. Phys. Lett., (1988). 9. K. Miyamoto, M. Sano, H. Kato, and T. Yao, Effects of ZnO/MgO Double Buffer Layers on Structural Quality and Electron Mobility of ZnO Epitaxial Films Grown on C- plane Sapphire, Jpn. J. Appl. Phys. Part 2, 41 L1203-L05 (2002). 10. S. K. Hong, Y. Chen, H. J. Ko, and T. Yao, Interface Engineering in ZnO Epitaxy, Phys. Stat. Sol. (b), (2002). 11. Y. Chen, S. K. Hong, H. J. Ko, V. Kirshner, H. Wenisch, T. Yao, K. Inaba, and Y. Segawa, Effects of an Extremely Thin Buffer on Heteroepitaxy with Large Lattice Mismatch, Appl. Phys. Lett., (2001). 12. V. Vashaei, T. Minegishi, H. Suzuki, T. Hanada, M.W. Cho, T. Yao, and A. Setiawan, Structural Variation of Cubic and Hexagonal MgxZn1-xO Layers Grown on MgO(111)/Csapphire, J. Appl. Phys., (2005). w wz

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