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1 Journal of the Korean Ceramic Society Vol. 44, No. 11, pp. 650~654, 007. Synthesis and Photoactivity of SnO -Doped TiO Thin Films Miewon Jung*, ** and Yunjung Kwak*, ** *Department of Chemistry, Sungshin Women s University, Seoul Korea **Institute of Basic Science, Sungshin Women s University, Seoul Korea (Received October 1, 007; Accepted November 3, 007) SnO ƒ v TiO w Ÿ z *, ** Á *, ** * w yw **» w ( ; ) ABSTRACT SnO -doped TiO thin films were prepared from tin (IV) bis (acetylacetonate) dichloride and titanium diisopropoxide bis (acetylacetonate) with pluronic P13 or degussa P5 as a structural-directing agent. These hydrolyzed sol were spin coated onto Si(100) wafer substrate. The microstructure, morphology and bonding states of thin films were studied by field-emission scanning electron microscopy (FE-SEM), X-ray diffractometry (XRD), and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity of these films was investigated by using indigo carmine solution. Key words : SnO -doped TiO, Pluronic P13, Degussa P5, XPS, Photoactivity 1. y œw x Ÿ TiO ˆ j SnO v j w w, w z. Ÿ 1) y ˆ f ƒ Ÿ w w, Ÿ w w - œ ƒ g Ÿ z w jš, ƒ Ÿ w y ùkü ˆ w ƒ w. TiO SnO v j - œ w z ƒ Ÿ y ˆ (Eg), š ù j» w t ƒ ƒ. SnO ƒ w û Ÿ z j, ù w j. ) ù, ˆ ƒ fv t y-y - œ k Corresponding author : Miewon Jung Tel : Fax : ù t w z ƒ k. Ÿ w j», t, ƒ š w w Ì ³ j» w w.» v œ, y,, yw, š - œ w gq. p - œ û 3) w k y w ù j» k j ³ wš k w w. w gq œ»q 4), j» gq p w, v, v š r p gq. vgq eƒ w»q z z w Ì w. w»œ j» v, t w»ƒ w» š. 5) ³ œ n w w» w» y» w t y ù š w ƒ w ù j» -» e ƒ ƒ w. - š w ƒ j 6) y y 650

2 SnO ƒ v TiO w Ÿ z 651 w j ³ w w y. ù Ÿ w xk l ƒ. w k w y ù j» k Ÿ w z w ƒ w. p œ w w, ƒ,, w.» ƒ š w pluronic P13 (P13)» ƒ ù j» TiO degussa P5 (P5) ƒƒ kw, w SnO ƒ v TiO w. y w k XRD XPS», xk Ì FE-SEM w. y indigo carmine (IC) kw UV-visible ŸŸ Ÿ w z r.. x Tin(IV) bis (acetylacetonate) dichloride 0.4 mmol titanium diisopropoxide bis (acetylacetonate) 16 mmol k -v q ƒƒ yww HCl ƒw (ph.5), 1h g. 3 g TiO degussa P5 (50 ±15 m /g;10~0% rutile+80~90% anatase;s³ j» 1 nm) 0.34 mmol P13 (H(-OCH CH -) 0 [-OCH(CH 3 )CH } 70 (-OCH CH -) 0 OH) (molecular weight 5,800) ƒƒ -v q 100 ml ƒw, 80 o C 6h y g ³ w. w Si(100) wafer 3600 rpm z 1 w, 75 o C 10 4z w w. 5 o C/min» 700 o C ƒ ƒ 1h w z, 1 (10 10 mm) 5 ppm indigo carmine ƒw, UV lamp (Philips, 53 nm, 0 W 3)w Ÿ w x w. y X- z»(x-ray Diffractometer, Bruker D8 Focus) CuKa, 40 kv, 40 ma, =0~80 o, scan step 0.0 o š scan time s ww. t, yw w k» w X- Ÿ Ÿ (X-ray Photoelectron Spectroscopy, PHI 5800 ESCA) w d w. j», s š Ì x (Field-Emission Scanning Electron Microscopy, HITACHI S-400) w 100,000 d w š, w Ÿ Ÿ (UV-visible spectroscopy, Sinko UV 100) w w. 3. š TiO ùk e p š p, ùk p ƒ ƒ ù. ùk p 400 C o 100 C w w o,, w ƒ w j w. ƒ 7) Non P5 P13 ƒ k XRD w Fig. 1(a) ùkü, t PEG(polyethylene glycol) wì w. ƒ w ù P5 ƒ k 8) Fig. 1. (a) X-ray diffraction patterns of SnO -doped TiO films with Non, P5, PEG, and P13 obtained after heattreated at 700 o C and (b) photodegradation curves of indigo carmine solution with different thin films. 44«11y(007)

3 65 Á Fig.. XPS spectra of (a) total (b) O (c) Sn and (d) Ti-binding energies of SnO -doped TiO thin films with P13. ùk (101) vj, PEG P13 ƒ g ùk p ƒ yw ùkù. Fig. (a), (b), (c) (d) P13 ƒ k w XPS rp. (a), O š e rp l w 58~53.5 ev yw w kƒ w, vq w (b) r 59.5, š ev 3ƒ vjƒ ev vj TiO (O L :Ti-O) w ùkù, ev vj w w» (OH) w, š ev vj» Si wafer wwš w w ùkù. 9) Fig. (c) (d) Sn 3d Ti p w vj ƒƒ ev, Sn Ti +4 k w w. Sn w Sn 4+ SnO j l k TiO ³ w s». 700 o C w 100,000 w FE-SEM Fig. 3(a) (f)¾ ùkü. t (a) (b), š (c) ³ ƒ š ƒ yw w š. s³ j» r, Non ƒ 30 nm, P5 0 nm, š P13 ƒ k 10 nm, P13 ƒ g ƒ j»ƒ ƒ š w. (d) (e), š (f), ƒ w 100 nm, P5 w 150 nm š P13 w Ì 350 nm. P13 š w ƒ ƒ Ë š ³ w gq w. j š ƒ û š P13 w ƒ w k š, Ì w ƒ k.» t w œw y Ë, w wz

4 SnO 가 도핑된 TiO 박막의 합성 및 광촉매 효과 653 조 내에서 촉매 개시 점 을 만들기 때문이라고 하였다. 또한 코팅 전에 알콕사이드 졸에 다공성 자리를 제공할 수 있는 고분자를 가하면, 열처리 시 고분자가 태워지면 서 입사광을 효율적으로 함유할 수 있는 빈자리를 만들 어 광촉매 효과를 증진시킨다. TiO 가 함유된 복합 산 화물 박막의 광학 활성도는 입자 크기, 빈 구멍, 결정상 의 구조, 표면적 및 표면의 거칠기 등 그 변수가 다양하 며 복합적으로 작용하므로 이에 대한 다각적인 연구가 필 요하다. 11) 4. 결 론 고분자 첨가제로 pluronic P13를, 무기 첨가제로 degussa P5를 사용하여 균일하고 조밀하게 증착된, SnO 가 도핑된 TiO 박막을 제조하여 광촉매 활성을 비교하 였다. 첨가제를 이용하면 박막을 균일하고 두껍게 제조할 수 있어 광촉매로서의 활성도가 증가하는데, 특히 분자량 이 큰 P13를 사용했을 때 더 효율적이었다. 이들 박막 내의 결합 상태는 Sn의 주 결합이 Sn 로써, SnO 클러 스터 상태로 TiO 결정 사이에 균일하게 분포되어있음을 알 수 있었다. 4+ Acknowlengement Fig. 3. FE-SEM micrographs of surface (a) Non (b) P5 (c) 이 연구는 006학년도 성신여자대학교 학술 연구 조성 비 지원에 의하여 연구되었으며 이에 감사드립니다. 후에도 조밀하게 결정화되어 균열 없는 박막을 얻을 수 있었다. 5 ppm의 indigo carmine (IC)용액에 각각의 박막들을 첨 가하여 광분해 효과를 관찰한 뒤, 분해 시간에 따른 상대 농도의 변화를 Fig. 1의 (b)에 나타내었다. IC의 주된 흡 수 피크는 600 nm 근처에서 나타나는데, 화합물에 존재 하는 하나의 C=C 이중결합과 개의 NH 및 개의 CO 기능기를 포함하는 발색단에 의한 것으로, 조사시간에 따 라 광분해가 일어나 피크의 세기가 감소하게 된다. Non, P5 그리고 P13의 순서로 분해 효과가 높았으며, P13 를 첨가제로 사용한 박막이 가장 효율적이었다. Fig. 1의 XRD 결과를 보면 P13를 첨가시킨 박막은 아나타제와 루틸의 혼합된 상이 나타나는데, 결정의 크기와 상전이도 뿐 아니라 여러 변수에 의해 광촉매 활성도가 조절되지 만, 아나타제 구조의 단일 상보다는 아나타제와 루틸의 혼합 상을 지니는 박막의 광분해 효율이 높다고 알려져 있다. 혼합된 상을 지닐 때의 향상된 광촉매 활성도에 대해서는 아직 논의 중이지만, 혼합된 상에서의 루틸구조 는 광촉매 활성을 가시광선 영역까지 연장시켜주는 안테 나 역할을 하며, 동시에 유사한 크기를 갖는 TiO 결정 구 REFERENCES P13 and cross section of (d) Non (e) P5 (f) P13, respectively. 4) 10) 1. J. C. Yu, L. Zhang, and W. Ho, Enhancing Effects of Water Content and Ultrasonic Irradiation on the Photocatalytic Activity of Nano-sized TiO Powders, J. Photochem. Photobio., A (00).. L. Zhang, Y. Zhu, Y. He, and W. Li, Preparation and Performances of Mesoporous TiO Film Photocatalyst supported on Stainless Steel, Appl. Catalysis B, (003). 3. Y. Takahashi and Y. Matsuoka, Dip-coating of TiO Films using a Sol derived from Ti(O-i-Pr) -diethanolamine-h O-iPrOH System, J. Mater. Sci., (1988). 4. G. A. Battiston, R. Gerbasi, and G. A. Rizzi, PECVD of Amorphous TiO thin Film: Effect of Growth Temperature and Plasma Gas Composition, Thin Solid Films, (000). 5. Y. K. Ree and J. C. Cha, Glass Transition Temperature of Poly (tert-butyl methacrylate) Langmuir-Blodgett Film and Spin-Coated Film by X-ray Reflectivity and Ellipsometry, Langmuir, 16 [5] (000). 6. D. Zao, J. Feng, Q. Huo, N. Melsh, and G. D. Stucky, Triblock Copolymer Syntheses of Mesoporus Silica with Periodic 50 to 300 Angstrom Pores, Science, 제 44 권 제 11호(007)

5 654 Á (1998). 7. R. A. Eppler,G Effect of Antimony Oxide on the Anatase- Rutile Transformation in Titanium Dioxide, J. Am. Ceram. Soc., 70 [4] C64-6 (1987). 8. M. W. Jung and Y. J. Kwak, Synthesis and Photoactivity of SnO -doped Anatase Type TiO Powder via Polymerization- Complex Route(in Korean), J. Kor. Ind. Eng. Chem., 17 [5] (006). 9. D. C. Hurum, A. G. Agrios, and K. A. Gray, Explaining the Enhanced Photocatalytic activity of Degussa P5 Mixed- Phase TiO using EPR, J. Phys. Chem. B, (003). 10. G. Balasubramanian, D. D. Dionysiou, M. T. Suidan, J. M. Laine, and I. Baudin, Evaluating the Activities of Immobilized TiO Powder Films for the Photocatalytic Degradation of Organic Contaminants in Water, Appl. Catalysis B, (004). 11. N. G. Park, K. M. Kim, M. G. Kang, K. S. Ryu, S. H. Chang, and Y. J. Shin, Chemical Sintering of Nanoparticles: A Methodology for Low Temperature Fablication of Dye-Sensitized TiO Films, Adv. Mater., (005). w wz

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