75 anatase and rutile phases approximately at ratio of 70:30. The surface porosity and
crystallite size plays a role in achieving the anatase phase. iii.
Through XRD calculation of Scherrer equation and comparison with the SEM images, the crystallite size for glass and stainless steel remained similarly the same,
which is the range of 27 – 32 nm. While for AP, the anatase crystal was only shown in the thin film that was calcined at 160 °C. It is safe to say that the anatase crystal
did not aggregated during the sol gel process but rather than during the calcinations of the thin film.
The acidic solution may have an effect to the metallic substrate as it may lead to corrosion; therefore, it is recommended that this sol gel is modified to have a neutral pH in order to be
able to be deposited onto different types of metallic substrates.
6.2 Recommendation
This project can be improved through these three steps: i.
The sol gel dipping method can be improved by increasing the thickness of the thin film on the substrates through consecutive coatings up until 10-12 layers. In most
studies, especially for glass and AP substrates, the coatings were performed in the range of 10-12 coatings in order to increase the film thickness.
ii. In addition, a further study should focus on the crystallite transformation during the
sol gel formulation. The anatase phase in AgTiO
2
sol gel can be enhanced with the hydrolysis increased at magnetically stirring at thermal temperature of 60-70°C in
order to inhibit the crystallization transformation under the heating condition. Then the sol gel can be deposited onto polymers as the substrates need not go through
higher temperature of calcinations.
76 iii.
The future works of this project may lead to the study of the photocatalytic and antimicrobial test of the AgTiO
2
thin film as the photocatalytic depended on the crystallite phases and sizes, surface porosity and surface areas. Furthermore, the
existence of AgTiO
2
will help to reduce the microbial activity by measuring the performance in the antimicrobial test.
77
7 References
Atabaki, M. M., Jafar, R. Idris, J., 2010. Sol–Gel Bioactive Glass Coating For Improvement Of Biocompatible Human Body Implant. Association of Metallurgical
Engineers of Serbia .
Barati, N., Sani, M. F., Ghasemi, H. Sadeghian, Z., 2009. Preparation of uniform TiO
2
nanostructure film on 316L stainless steel by sol-gel dip coating. Applied Surface Science, Volume 255, p. 8328–8333.
Brundle, C. R., Charles A. Evans, J., Wihon, S. Fitzpatrick, L. E., 1992. Encyclopedia of Materials Characterization: Surfaces, Interfaces, Thin Films.
Stoneham, MA : Butterworth- Heinemann .
Chen, Q., Liu, H., Ye, R. Lu, J., 2008. Ag-doped antibacterial porous materials with slow release of silver ions. Journal of Non-Crystalline Solids, Volume 354, p. 1314–1317.
Cullit, B., 1987. Elements of X-ray Diffraction. 2nd ed. USA: Addison-Welley Publishing Company.
Duminica, F., Maury, F. Hausbrand, R., 2009. Effect of H
2
on the Microstructure and Properties of TiO
2
Films Grown by Atmospheric Pressure MOCVD on Steel substrates. ECS Transactions,
258, pp. 249-256. Eshaghi, A., Pakshir, M. Mozaffarinia, R., 2010. Photoinduced properties of
nanocrystalline TiO
2
sol gel derived thin films. Bull. Mater. Sci., 334, p. 365–369. Falaras, P., Xagas, A., Androulaki, E. Hiskia, A., 1999. Preparation, fractal surface
morphology and photocatalytic properties of TiO
2
films. Thin Solid Films , Volume 357, pp. 173-178.
Ibrahim, S. M., Negishi, N., Masrom, A. K. Mazinani, B., 2012. TiO
2
Transparent Thin Film for Eliminating Toluene. ISRN Nanotechnology.
Ito, S., Takeuchi, T., Katayama, T. Kitamura, T., 2003. Conductive and Transparent Multilayer Films for Low-Temperature-Sintered Mesoporous TiO
2
Electrodes of Dye- Sensitized Solar Cells. American Chemical Society; Chemical Material, Volume 15, pp.
2824-2828.
Madina, V., Read, S., Grundmeier, G. Ghosh, S., 2010. Development and evaluation of coatings and surface conditions on steel for antibacterial and easy-to-clean properties,
Luxermboug: Publications Office of the European Union.
Murali, K., 2007. Properties of sol-gel dip-coated zinc oxide thin films. Journal of Physics and Chemistry of Solids,
Volume 68, pp. 2293-2296.
78 Neti, N. R. Joshi, P., 2010. Cellulose reinforced-TiO
2
photocatalyst coating on acrylic plastic for degradation of reactive dyes. Journal of Coating Technology Research, 75, p.
643–650.
Ohno, T., Sarukawa, K., Tokieda, K. Matsumura, M., 2001. Morphology of a TiO
2
Photocatalyst Degussa, P-25 Consisting of Anatase and Rutile Crystalline Phases. Journal of Catalysis,
Volume 203Issue 1, p. Pages 82–86. Ohtani, B., Prieto-Mahaney, O. O., Li, D. Abe, R., 2010. What is Degussa Evonik P25?
Crystalline composition analysis, reconstruction from isolated pure particles and photocatalytic activity test. Journal of Photochemistry and Photobiology A : Chemistry,
2162-3, pp. 179-182 .
Paez, L. R. Matoušek, J., 2004. Properties of sol-gel TiO
2
layers on glass substrate. Ceramics − Silikáty,
482, pp. 66-71. Page, K., Parkin, I. P. Wilson, M., 2009. Photocatalytic Thin Films; Their
Characterizations and Antimicrobial Properties. University College of London: University
College of London. Porter, J., Li, Y. Chan, C., 1999. J. Mater. Sci., Volume 34, p. 1523.
Seery, M., Nolan, N. Pillai, S., 2009. Spectroscopic Investigation of the Anatase-to- Rutile Transformation of Sol-Gel Synthesised TiO
2
Photocatalysts. Centre for Research in Engineering Surface Technology .
Sisti, L., Cruciani, L., Vannini, M. Berti, C., 2012. TiO
2
deposition on the surface of activated fluoropolymer substrate. Thin Solid Films, Volume 520, p. 2824–2828.
Sondi, I. Salopek-Sondi, B., 2004. Silver nanoparticles as antimicrobial agent: a case study on E. coli as a model for Gram-negative bacteria. Journal of Colloid and Interface science,
2751, pp. 177-182.
Spurr, R. A. Myers, H., 1957. Quantitative analysis of anatase–rutile mixtures with an X- ray diffractometer. Analytical Chemistry, 295, p. 760–762.
Sun, S.-Q., Sun, B., Zhang, W. Wang, D., 2008. Preparation and antibacterial activity of AgTiO
2
composite film by liquid phase deposition LPD method. Bull. Material Science, 31No.1, Indian Academy of Sciences., p. 61–66.
Su, W., Wang, S. W., Fu, X. Weng, J., 2010. Plasma pre-treatment and TiO
2
coating of PMMA for the improvement of antibacterial properties. Surface Coatings Technology,
Volume 205, p. 465–469.
79 TIGER Drylac®, A. P. C., 2011. Tiger DryLac Coatings. [Online] Available at:
http:www.tiger-coatings.comfileadminuser_uploaddownloadareadeProduktfolderAM- Folder_0311_low_01.pdf [Accessed 16th May 2012].
Viana, M. M. Mohallem, N. D. S., 2009. Synthesis and Characterization of AgTiO
2
Nanocomposite Thin Films. Hawaii, ICCE Proceedings.
Wang, G., Xu, L., Zhang, J. Yin, T., 2012. Enhanced Photocatalytic Activity of TiO
2
Powders P25 via Calcination Treatment. International Journal of Photoenergy. Yao, M., Chen, J., Zhao, C. Chen, Y., 2009. Photocatalytic activities of Ion doped TiO
2
thin films when prepared on different substrates. Thin Solid Films, Volume 517, p. 5994– 5999.
You, X., Zhang, F. C. Jinlong, 2005. Effects of Calcination on the Physical and Photocatalytic Properties of TiO
2
Powders Prepared by Sol–Gel Template Method. Journal of Sol-Gel Science and Technology,
Volume 34, p. 181–187. Yuan, C. Hu, Y., 2006 . Low-temperature Preparation of Photocatalytic TiO
2
Thin Films on Polymer Substrates by Direct Deposition from Anatase. J. Mater. Sci. Technology, 222,
p. 239.
Yuna, Y. J., Chunga, J. S., Kima, S. Kim, E. J., 2004. Low-temperature coating of sol–gel anatase thin films. Materials Letters, Volume 58, p. 3703– 3706.
Zaleska, A., 2008. Doped-TiO
2
: A Review. Recent Patents on Engineering, 23, pp. 157- 164.
80
8 Appendix
Figure 8.1: Glancing angle XRD pattern of AgTiO
2
thin film on glass – calcined at 200 °C
Figure 8.2: Glancing angle XRD pattern of AgTiO
2
thin film on glass – calcined at 400 °C
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
Counts
2000 4000
6000 G 200
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
Counts
2000 4000
6000 G 400b
81
Figure 8.3: Glancing angle XRD pattern of AgTiO
2
thin film on glass – calcined at 600 °C
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
Counts
2000 4000
6000 G 600a
82
Figure 8.4: Glancing angle XRD pattern of AgTiO
2
thin film coated onto Acrylic Perspex calcined at 160 °C
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
unts
10000 20000
30000 40000
AP 160 C b
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
unts
10000 20000
30000 AP 120b
83
Figure 8.5: Glancing angle XRD pattern of AgTiO
2
thin film coated onto Acrylic Perspex calcined at 120 °C
Figure 8.6: Glancing angle XRD pattern of AgTiO
2
thin film on stainless steel – calcined at 200 °C
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
Counts
2000 4000
6000 8000
SS 200a W-O RT
84
Figure 8.7: Glancing angle XRD pattern of AgTiO
2
thin film on stainless steel – calcined at 400 °C
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
Counts
2000 4000
6000 8000
SS 400a W-O RT
85
Figure 8.8: Glancing angle XRD pattern of AgTiO
2
thin film on stainless steel – calcined at 600 °C
Position [°2Theta] Copper Cu 20
30 40
50 60
70 80
Counts
5000 10000
SS 600 W-O RT
86
Table 3: XRD phase transition calculation Samples
IR IA
X Y
Crystallite Size
FHWM 2
cos SS_200wo
511.98 1021.14
61.19027104 38.52683288
27.29320871 0.2952
0.00515288 25.317
12.6585 0.975694
SS_400wo 365.7
1040.35 69.22004936
30.52638608 27.28804648
0.2952 0.00515288
25.2203 12.61015
0.975878 SS_600wo
430.71 526.33
49.13561764 50.56623001
32.75867684 0.246
0.004294067 25.4231
12.71155 0.97549
G_200 253.48
772.57 70.6690735
29.08428338 27.29310173
0.2952 0.00515288
25.315 12.6575
0.975697 G_400
225.76 965.41
77.17128523 22.619248
27.29267388 0.2952
0.00515288 25.307
12.6535 0.975713
G_600 253.94
1230.89 79.30358146
20.50131918 32.7524283
0.246 0.004294067
25.326 12.663
0.975676 AP_120
DIV0 DIV0
1 AP_160
1120.71 100
DIV0 81.8725715
0.0984 0.001717627
25.273 12.6365
0.975778 TiO2 Powder, 60
158.62 306.92
60.46799454 39.24722137
160.4565851 0.0502
0.000876269 25.1878
12.5939 0.97594
TiO2 Powder, 600 126.83
313.9 66.17616754
33.55734886 68.79817049
0.1171 0.002044046
25.2733 12.63665
0.975777 Ceramic Glass
592.02 933.11
55.47571416 44.22984398
96.36176535 0.0836
0.001459284 25.2465
12.62325 0.975828
Glazed Ceramic 509.6
1014.3 61.14130435
38.57566766 98.71948483
0.0816 0.001424373
25.2253 12.61265
0.975869 Non-glazed ceramic
270.84 1364.03
79.92475988 19.88452819
53.50076935 0.1506
0.002628807 25.3335
12.66675 0.975662