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
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