Preparation Development of High Photocatalyst Nanotubes from Thai Ilmenite Mineral by Hydrothermal Method

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1 Preparation Development of High Photocatalyst Nanotubes from Thai Ilmenite Mineral by Hydrothermal Method 1, 2, 3 4,* 1, 2, 3, 4.,., Thanakorn Wirunmongkol 1 Narongchai O-Charoen 2 Kullawadee Sungsanit 3 Sorapong Pavasupree 4,* 1, 2, 3, 4 Department of Materials and Metallurgical Engineering, Faculty of Engineering, Rajamangala University of Technology Thanyaburi, Klong 6, Thanyaburi, Pathumthani 12110, Thailand Tel.: , fax: , sorapongp@yahoo.com * (TiO 2 ~ 65.40%, Fe 2 O 3 ~ %) ºC 24 (XRF), (XRD), (SEM), (TEM) Fe 2 O wt% H 2 Ti x O 2x (P-25, JRC-01, JRC-03 White pigment) Abstract The aims of this research were to development of high photocatalyst nanotubes from Thai ilmenite mineral (TiO 2 ~ %, Fe 2 O 3 ~ %) prepared by hydrothermal method. Nanotubes derived from washed ilmenite mineral with 10 M NaOH aqueous solution (five times) before synthesized via simple hydrothermal method at 105 ºC for 24 h. The prepared samples were characterized by X-ray fluorescene (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The quantities of Fe 2 O 3 in the prepared samples decreased from to wt%. The crystalline structure of the as-synthesized sample demonstrated a layered titanate form, H 2 Ti x O 2x+1. The length of the prepared nanotubes ranged from nm with an average inner diameter around

2 6-8 nm and outer diameter around nm. Additionally, photocatalytic activities of the prepared samples have been found to be higher than those of commercially grade nanoparticles TiO 2 (P-25, JRC- 01, JRC-03, and white pigment). Keywords: nanotubes, ilmenite, hydrothermal, photocatalytic activity. 1. (TiO 2 ) 1 (One-dimentional nanostructures) (nanowires), (nanorods), (nanotubes) (nanofibers) [1], [2], [3] [4] TiO 2 (metal oxide) [5], [6], [7], [8], [9, 10],, [11-14] TiO 2 (Low-dimentional) - (Sol-gel), (Elec-trodeposition) (Electrospinning) (Hydrothermal) [2, 13-18] Kasuga [17, 18] [19-21, 24] (FeTiO 3 ) TiO 2 ( 50-60%) (leucoxene) (ilmenite) [24, 25] (~ / ) , (D.I. water) - (ph)

3 1, ºC 24 (Magnetic bar) 0.1 (Deionized water: DI) ºC (BET Specific surface area) (XRF) (XRD) (SEM) (TEM) The Brunauer-Emmett- Teller (BET) 2.3 (Photocatalytic activity) I - 3 I - I 2 I I - I 2 + 2e - (1) I 2 + I + - I 3 (2) Potassium Iodide (KI) UV 365 nm 15 W 1 (Centrifuge) nm UV-visible spectrophotometer (UV-1601 SHIMADZU) UV-visible spectrophotometer - I 3 ( ) 3. (a) (b) (c) 2 a) b) NaOH 5 c)

4 3.1 NaOH 5 2a 2b (Fe) NaOH HCl [20] 1 Oxide Ilmenite As-synthesized As-synthesized (%wt) (Previous work) (This study) TiO Fe 2 O Al 2 O SiO MnO ZrO MgO Cr 2 O P 2 O SO Y 2 O ZnO Nb 2 O CaO SnO Cl F < Fe 2 O 3 NaOH %wt TiO 2 NaOH %wt [20, 25] Fe 3+ (visible spectrum) (band gap energy) [27-29] (Rutile) (H 2 Ti x O 2x+1 ) trititanate (H 2 Ti 3 O 7 ) [19-21, 24] (NaCl) NaOH Na + As-synthesized Ilmenite mineral XRF 1 Fe 2 O 3, Al 2 o 3, SiO 2, MnO Fe 2 O 3 NaOH 3 (XRD patterns) (H = hydrogen titanate R = rutile TiO 2 )

5 3.3 SEM NaOH 5 4 NaOH 1-10 m ( 4a) NaOH m ( 4b) SEM 5 TEM 6 5 SEM 10,000 (a) (a) (b) 50 nm (b) (c) 6 TEM (a) 40,000 (b) 285,000 4 SEM (a) (b) NaOH (c) NaOH 5 TEM

6 S. Pavasupree [24] A. Simpraditpan [25, 26] T. Kasuga [17, 18] nm nm (BET-specific surface area) BET surface area (m Samples 2 /g) Ilmenite mineral ~ 0 Nanofibers titanate (previous work) [20-21] Nanotubes titanate (previous work) Nanotubes titanate (this study) Commercial nano TiO 2 (P- 25) BET / / ( ) 3 (~49. / ) [24-26] [17-19, 22-23] TiO 2 (P-25) 50. / I - 3, TiO 2 (P-25, JRC-01, JRC-03 white pigment) 3.5, TiO 2 7 NaOH,, TiO 2 P-25, JRC-01, JRC-03, (White pigment) I 3 - KI 0.2 M 10 ml UV 1 NaOH I M, TiO 2 P-25, JRC-01, JRC-03, (White pigment) I , , , , M TiO 2

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