Malaysian Journal of Analytical Sciences Vol 22 No 2 (2018): 333 - 338

DOI: 10.17576/mjas-2018-2202-20

 

 

 

Characterization of TiO2 Thin Films Derived using Acetic Acid and Nitric Acid

 

(Pencirian Filem Nipis TiO2 yang Dihasilkan Menggunakan Asid Asetik dan Asid Nitrik)

 

Nur Munirah Safiay1, Syahman Shamsuddin2, Nur Najwa Yunus2, Fazlena Hamzah2*

 

1Centre of Nanoscience and Nonaotechnology, Institute of Science

2Biocatalysis and Biobased Material Research Group, CoRe of Green Technology & Sustainable Development, Faculty of Chemical Engineering

Universiti Teknologi MARA, Shah Alam Campus, 40450 Shah Alam, Selangor, Malaysia

 

*Corresponding author:  fazlena@salam.uitm.edu.my

 

 

Received: 15 February 2017; Accepted: 2 January 2018

 

 

Abstract

Titanium dioxide (TiO2) thin films were prepared via sol gel method using different concentration of glacial acetic acid and nitric acid. The deposition of TiO2 gel on the ITO substrate was conducted using spin coating techniques at a rate of 3,000 rpm for 30 s and was calcinated at 500 oC for 10 minutes. The study was conducted to determine the surface morphology and characteristic of the TiO2 thin film based on the different acid precursor. The GAA – TiO2 and HNO3 - TiO2 thin film were analyzed using Contact Angle Goniometer for absorption property study and Scanning Electron Microscope (SEM) for surface topography study. The result indicated that different acid and different concentration influence wettability of the synthesized TiO2 thin film. Higher concentration of GAA results in higher contact angle of TiO2 thin film whereas higher concentration of HNO3 reduced the contact angle of TiO2 thin film. However, the contact angle obtained through this study was in a range of 27.55o – 67.55o for the concentration acid of 8 – 10 mmol which represent hydrophilic characteristic of the TiO2 thin film. For surface analysis, uneven and not uniform surface of thin film was detected for the entire sample. This might be due to the several factors such as temperature and particle size that limited the adhesion of the TiO2 sol gel to the ITO substrate. Transform Infrared Spectroscopy (FTIR) analysis was used to validate the present of the Ti-O bond vibrations in the sample and it was observed in ranges of 515–800 cm−1. On the other hand, the crystallinity structure of the synthesized TiO2 was validated using X-ray Diffraction (XRD). The results indicated that both GAA - TiO2 and HNO3 - TiO2 mixtures gave a strong anatase crystal structure. The major XRD diffraction peaks can be attributed to (101), (004), (200), (211), (204) and (116) plane of the tetragonal TiO2-anatase phase.

 

Keywords:  characterization, acid, thin films, titanium dioxide, titanium isopropoxide

 

Abstrak

Titanium dioksida (TiO2) filem nipis telah dihasilkan melalui kaedah sol gel dengan menggunakan kepekatan asid asetik glasial dan asid nitrik yang berbeza. Pemendakan gel TiO2 pada substrat ITO dilakukan menggunakan teknik salutan berputar pada kadar 3,000 rpm selama 30 s dan dikalsinasi pada 500 oC selama 10 minit. Kajian ini dijalankan untuk menentukan morfologi permukaan dan ciri-ciri filem TiO2 nipis berdasarkan kepekatan asid yang berbeza. Filem nipis GAA - TiO2 dan HNO3 - TiO2 dianalisis dengan menggunakan goniometer sudut sentuh untuk kajian ciri-ciri penyerapan dan mikroskop imbasan elektron (SEM) untuk kajian topografi permukaan. Hasil kajian menunjukkan bahawa asid yang berbeza dan kepekatan yang berbeza mempengaruhi kelembapan TiO2 filem nipis yang dihasilkan. Kepekatan GAA yang tinggi menghasilkan sudut sentuh yang lebih tinggi pada TiO2 filem nipis manakala kepekatan HNO3 yang lebih tinggi mengurangkan sudut sentuh TiO2 filem nipis. Walau bagaimanapun, sudut hubungan yang diperolehi melalui kajian ini adalah dalam lingkungan 27.55o - 67.55o untuk kepekatan asid 8 - 10 mmol yang mewakili ciri hidrofilik TiO2 filem nipis. Untuk analisis permukaan, permukaan filem nipis adalah tidak rata dan tidak seragam dikesan untuk semua sampel. Hal ini mungkin disebabkan beberapa faktor seperti suhu dan saiz zarah yang menghadkan pelekatan sol gel TiO2 kepada substrat ITO. Analisis Spektroskopi Inframerah (FTIR) digunakan untuk mengesahkan kehadiran getaran Ti-O di dalam sampel dan keputusan menunjukkan kehadiran getaran Ti-O di dalam lingkungan 515-800 cm-1. Manakala struktur kristal TiO2 yang disintesis telah disahkan dengan menggunakan pembelauan sinar-X (XRD). Keputusan menunjukkan bahawa campuran GAA - TiO2 dan HNO3 - TiO2 memberikan struktur kristal anatase yang kuat. Puncak pembelauan XRD yang utama boleh dikaitkan dengan fasa TiO2-anatase tetragonal pada (101), (004), (200), (211), (204) dan (116).

 

Kata kunci:  pencirian, asid, filem nipis, titanium dioksida, titanium isopropoksida

 

References

1.       Titanium dioxide definition, https://en.wikipedia.org/wiki/Titanium_dioxide [Access online 20 October 2016].

2.       Hoffmann, M. R., Martin, S. T., Choi, W. and Bahnemann, D.W. (1995). Environmental applications of semiconductor photocatalysis. Chemical Reviews, 95: 69-96.

3.       Kajitvichyanukula P., Ananpattarachaia J. and Pongpom S. (2005). Sol–gel preparation and properties study of TiO2 thin film for photocatalytic reduction of chromium(VI) in photocatalysis process. Science and Technology of Advanced Materials, 6: 352-358.

4.       Qiu J., Zhang S. and Zhao H. (2011). Recent applications of TiO2 nanomaterials in chemical sensing in aqueous media. Sensors & Actuators: B. Chemical, 160: 875-890.

5.       Ding Z., Hu X., Yue P. L., Lu G. Q. and Greenfield P. F. (2001). Synthesis of anatase TiO2 supported on porous solids by chemical vapor deposition. Catalysis Today, 68: 173-182.

6.       Pecchi G., Reyes P. and Sanhueza, J. P. (2001). Photocatalytic degradation of pentachlorophenol on TiO2 sol–gel catalysts. Chemosphere, 43: 141–146.

7.       Sonawane, R. S., Hegde, S. G. and Dongare, M. K. (2002). Preparation of titanium (IV) oxide thin film photocatalyst by sol–gel dip coating. Materials Chemistry and Physics, 77: 744–750.

8.       Sakka, S., Yoko, T. in: Jørgenson, J. C. and Reisfield, R. (Eds.) (1991). Chemistry, spectroscopy, and application of sol–gel glasses, Springer, Heidelberg: 89–91.

9.       Miao, D., Hu, H., Li, A., Jiang, S. and Shang, S. (2015). Fabrication of porous and amorphous TiO2 thin films on flexible textile substrates. Ceramics International, 41: 9177-9182.

10.    Li, Y. G., Ma, L. X., Sarro, P. M., Du, D. X. and Liu, X. F. (2016). Mass sensitivity of aluminum nitride thin film based surface acoustic wave sensors prepared for biosensing application. Symposium on Piezoelectricity, Acoustic Waves, and Device Applications, 21-24 Oct. 2016.

11.    Alzamani, M., Shokuhfar, A., Eghdam, E. and Mastali, S. (2013). Influence of catalyst on structural and morphological properties of TiO2 nanostructured films prepared by sol–gel on glass. Progress in Natural Science: Materials International, 23(1):77–84.

12.    Parra, R., Góes, M. S., Castro, M. S., Longo, E., Bueno, P. R. and Varela, J. A. (2008). Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid. Chemistry of Materials, 20: 143-150.

13.    Gonzalez, R. J., Zallen, R. and Berger, H. (1997). Infrared reflectivity and lattice fundamentals in anatase TiO2s. Physic Review B, 55: 7014-7017.

14.    Nolan, N. T., Seery, M. K. and Pillai, S. C. (2009). Spectroscopic investigation of the anatase-to-rutile transformation of sol-gel-synthesized TiO2 photocatalysts. Journal of Physical Chemistry C, 2113: 16151-16157.

15.    Gökdemir, F. P., Yüzbaşıoğlu, V. E., Keskin, B., Özdemir O. and Kutlu, K. (2014). Formation of TiO2 thin films by a modified sol gel route and characterization of structural, optical and electrochromic properties. Advance Materials Letter, 5(7): 367-371.

16.    Adamczyk, A. and Długoń E. (2012). The FTIR studies of gels and thin films of Al2O3 – TiO2 and Al2O3 – TiO2 – SiO2 systems. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 89: 11-17.

17.    Tsegaa, M. and Dejeneb, F. B. (2017). Influence of acidic pH on the formulation of TiO2 nanocrystalline powders with enhanced photoluminescence property. Heliyon, 3:246.

18.    Yu, J. C., Yu, J., Ho, W. K, Jiang, Z. and Zhang, L. Z (2002). Effects of F- doping on the photocatalytic activity and microstructures of nanocrystalline TiO2 powders. Chemistry of Materials, 14: 3808-3816.

19.    Serrano, D. P., Calleja, G., Sanz, R. and Pizarro, P. (2007). Development of crystallinity and photocatalytic properties in porous TiO2 by mild acid treatment. Journal of Materials Chemistry, 17(12): 1178-1187.

20.    Thamaphat, K., Limsuwan, P. and Ngotawornchai, B. (2008). Phase characterization of TiO2 powder by XRD and TEM Kasetsart Journal (Natural Science), 42: 357-361.

 




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