DOI QR코드

DOI QR Code

The Effect of Additives on the Preparation of Nanosized TiO2 Particles

나노크기 TiO2의 제조에 미치는 첨가제 영향

  • Kim, Seok-Hyeon (Department of Chemical Engineering, Pukyoung National University) ;
  • Na, Seok-En (Department of Chemical Engineering, Pukyoung National University) ;
  • Kim, Si-Young (Department of Mechanical System Engineering, Pukyoung National University) ;
  • Kim, Seong-Soo (Department of Environmental Administration, Catholic University of Busan) ;
  • Ju, Chang-Sik (Department of Chemical Engineering, Pukyoung National University)
  • 김석현 (부경대학교 화학공학과) ;
  • 나석은 (부경대학교 화학공학과) ;
  • 김시영 (부경대학교 기계시스템공학과) ;
  • 김성수 (부산 가톨릭대학교 환경행정학과) ;
  • 주창식 (부경대학교 화학공학과)
  • Received : 2013.04.16
  • Accepted : 2013.06.15
  • Published : 2013.08.01

Abstract

Nanosized $TiO_2$ particles were prepared from titanium (IV) sulfate solution using base solutions at low reaction temperature ($95^{\circ}C$) and atmospheric pressure by hydrothermal precipitation method without calcination. The effects of preparation conditions, such as kind of base solutions (NaOH, $NH_4OH$, Monoethanolamine, Diethanolamine, Triethanolamine) and surfactants (CTAB, Span 20, SDBS), concentration of surfactants, temperature and pH, on the physical properties of $TiO_2$ particles have been investigated by XRD, SEM and Zeta-potential meter. Absorption area was also investigated by DRS in order to confirm the photocatalytic activity of the nanosized $TiO_2$ particles. It was turned out that, among base solutions, NaOH provides the smallest $TiO_2$ particles with excellent crystallinity. And cationic surfactant (CTAB) prepared smaller $TiO_2$ particles than any other surfactants. When CTAB is added in the concentration ratio of $Ti(SO_4)_2$:CTAB=10:1, $TiO_2$ particles with particle diameter of 5.8 nm were prepared. This is approximately 1/10 of that prepared without CTAB.

비교적 낮은 온도와 상압에서 전구체 Titanium(IV) sulfate와 염기성 용액을 반응시키는 수열합성법을 이용하여 소성과정을 거치지 않고 $TiO_2$ 나노입자를 제조하였다. 염기성 용액의 종류(NaOH, $NH_4OH$, Monoethanolamine, Diethanolamine, Triethanolamine), 첨가되는 계면활성제의 종류(CTAB, Span 20, SDBS)와 농도, 제조 온도, pH 등을 변화시켜 $TiO_2$를 제조하였고, 생성되는 입자의 결정성, 입자크기 등과 같은 물리적 특성은 XRD, SEM, Zeta-potential 등을 사용하여 분석하였다. 또한, 광촉매적 특성을 확인하기 위하여 DRS를 통해 흡광면적을 측정, 비교하였다. 침전제로 사용된 염기성 물질 중 NaOH가 결정성이 우수하고 입자크기가 작은 $TiO_2$를 제조하는데 가장 효과적임을 확인할 수 있었다. 계면활성제는 양이온성 계면활성제인 CTAB를 첨가한 경우 다른 계면활성제보다 작은 크기의 $TiO_2$를 제조할 수 있었다. 그리고 동일한 조건에서 전구체인 $Ti(SO_4)_2$와 CTAB의 농도비를 10 : 1로 조절한 경우 CTAB를 첨가하지 않은 경우보다 제조되는 $TiO_2$ 입자의 크기는 약 1/10인 5.8 nm로 감소하였다.

Keywords

References

  1. Peng, T., Zhao, D., Dai, K., Shi, W. and Hirao, K., "Synthesis of Titanium Dioxide Nanoparticles with Mesoporous Anatase Wall and High Photocatalytic Activity," J. Phys. Chem. B, 109, 4947-4952(2005). https://doi.org/10.1021/jp044771r
  2. Wang, F., Shi, Z., Gong, F., Jiu, J. and Adachi, M., "Morphology Control of Anatase $TiO_{2}$ by Surfactant-assisted Hydrothermal Method," Chin. J. Chem. Eng., 15(5), 754-759(2007). https://doi.org/10.1016/S1004-9541(07)60158-X
  3. Cheng, H., Ma, J., Zhao, Z. and Qi, L., "Hydrothermal Preparation of Uniform Nanosize Rutile and Anatase Particle," Chem. Mater., 7, 663-671(1995). https://doi.org/10.1021/cm00052a010
  4. Lee, B. M., Shin, D. Y. and Han, S. M., "Synthesis of Hydrous $TiO_{2}$ Powder by Dropping Precipitant Method and Photocatalytic Properties," J. Korean Ceramic Soci., 37(4), 308-313(2000).
  5. Seo, D. S., Lee, J. K., You, H. G. and Kim, H., "Preparation of $TiO_{2}$ Nanocrystalline Powder at Low Temperature," Korean J. Ceramic Soci., 38(4), 331-336(2001).
  6. Chen, K., Li, J., Wang, W., Zhang, Y., Wang, X. and Su, H., "Effect of Surfactants on Microstructure and Photocatalytic Activity of $TiO_{2}$ Nanoparticles Prepared by the Hydrothermal Method," Mater. Sci. Semicond. Process, 15, 20-28(2012). https://doi.org/10.1016/j.mssp.2011.05.007
  7. Jung, M. W. and Kwak, Y. J., "Synthesis and Photoactivity of $SnO_{2}$-Doped Anatase-Type $TiO_{2}$ Powder via Polymerization-Complex Route," J. Korean Ind. Eng. Chem., 17(5), 561-564(2006).
  8. Wang, H., Liu, P., Cheng, X., Shui, A. and Zeng, L., "Effect of Surfactant on Synthesis of $TiO_{2}$ Nano-particles by Homogeneous Precipitation Method," Powder Technol., 188, 52-54(2008). https://doi.org/10.1016/j.powtec.2008.03.010
  9. Lee, M. S., Ju, C. S., Lee, G. D. and Hong, S. S., "Effect of the Water/ Surfactant Molar Ratio $(W_{0})$ on Synthesis of Nanosized $TiO_{2}$/$SiO_{2}$ by W/O Microemulsion and Their Photocatalytic Activity," Korean Chem. Eng. Res.(HWAHAK KONGHAK), 41(4), 432-438(2003).
  10. Liao, D. L. and Liao, B. Q., "Shape, Size and Photocatalytic Activity Control of $TiO_{2}$ Nanoparticles with Surfactants," J. Photochem. Photobiol. A-Chem., 187, 363-369(2007). https://doi.org/10.1016/j.jphotochem.2006.11.003
  11. Hidalgo, M. C., Aguilar, M., Maicu, M., Navio, J. A. and Colon, G., "Hydrothermal Preparation of Highly Photoactive $TiO_{2}$ Nanopartuicles," Catal. Today, 129, 50-58(2007). https://doi.org/10.1016/j.cattod.2007.06.053
  12. Na, S. E., Jeong, S. G., Jeong, G. S., Kim, S. Y. and Ju, C. S., "Preparation of Zinc Oxide by Hydrothermal Precipitaation and Degradation of Tartrazine," Korean Chem. Eng. Res.(HWAHAK KONGHAK), 49(6), 752-757(2011). https://doi.org/10.9713/kcer.2011.49.6.752
  13. Woo, S. H. and Kim, W. W., "Scale up Test of Ultrafine $TiO_{2}$ Powder by Homogeneous Precipitation Process at Low Temperatures," Trends in Metals & Mat. Eng., 19(3), 8-12(2006).
  14. Kim, S. Y., "Preparation, Characterization and Photocatalytic Activities of Titanium Dioxide Nanoparticles", Master degree, Department of Chemical Engineering, Chungbuk National University, Cheongju, Korea(2010).
  15. Kim, G. H., Lee, W. J., Kim, D. G., Lee, S. K., Lee, S. H. and Kim, I. S., "Synthesis of Nano-sized $TiO_{2}$ Powder Using a Hydrothermal Process," Korean J. Met. Mater., 48(6), 543-550(2010).

Cited by

  1. Core-Shell Composites Using Amphiphilic Graft Copolymer Template vol.52, pp.2, 2014, https://doi.org/10.9713/kcer.2014.52.2.209
  2. 주형합성을 통한 메조포러스 TiO2 제조 및 실리카 메조포어 내부에서의 TiO2 상전이 거동 변화 vol.56, pp.2, 2013, https://doi.org/10.9713/kcer.2018.56.2.261