Malaysian
Journal of Analytical Sciences Vol 20 No 2 (2016): 373 - 381
ELECTROCHEMICAL SYNTHESIS OF ORDERED TITANIA NANOTUBES
IN MIXTURE OF ETHYLENE GLYCOL AND GLYCEROL ELECTROLYTE
(Sintesis Nanotiub Titania Bertertib Secara
Elektrokimia dalam Campuran Elektrolit Etilena Glikol dan Gliserol)
Lim Ying Chin1*, Zulkarnain Zainal2,
3, Zuraida Khusaimi1, Siti Sarah Ismail1
1School
of Chemistry and Environment, Faculty of Applied Sciences,
Universiti Teknologi MARA, 40450
Shah Alam, Selangor, Malaysia
2Department
of Chemistry, Faculty of Science
3Advanced
Materials and Nanotechnology Laboratory, Institute of Advanced Technology
(ITMA)
Universiti Putra Malaysia, 43400
UPM Serdang, Selangor, Malaysia
*Corresponding author: limyi613@salam.uitm.edu.my
Received: 24
February 2015; Accepted: 27 October 2015
Abstract
The
electrolyte chemistry (nature and its composition) plays a critical role in
determining the nanotube architecture and its growth process. In the present
study, the formation of well-ordered titania nanotubes (TNT) is achieved by
electrochemical anodization of titanium substrate in aqueous ethylene glycol-glycerol
electrolyte (EG/Gly). The resulted samples were characterized using X-ray Diffraction (XRD) and
the morphology changes were monitored by Field Emission Scanning Electron
Microscopy (FESEM). Compositional changes of the titania nanotubes (TNT) were
determined using Energy Dispersive X-ray Spectroscopy (EDX). The influence of
anodization voltage, volume ratio of electrolyte and NH4F content on
the morphology and geometry of titania nanotubes have been investigated. The
nature of electrolytes influenced the ordering and uniformity of nanotubes. In
addition, nanotubes with various diameters ranging from 62 – 112 nm and lengths
of 1.1 – 1.3 μm were obtained by controlling the anodization voltage and volume
ratio of EG/Gly. Ultimately, anodization of Ti at 20 V in 1:1 volume ratio of EG/Gly
containing 0.25 – 1.0 wt.% NH4F appears to be an optimum condition
for controlling the ordering of nanotubes.
Keywords: titania, nanotube,
anodization, glycerol, ethylene glycol
Abstrak
Kimia
elektrolit (sifat dan komposisinya) memainkan peranan kritikal dalam menentukan
senibina nanotiub dan proses pertumbuhannya. Dalam kajian ini, pembentukan nanotiub
titania (TNT) tertertib rapi boleh dicapai melalui penganodan subtrat titanium
secara elektrokimia dalam larutan akueus etilena glikol-gliserol (EG/Gly).
Pencirian sampel dilakukan menggunakan pembelauan sinar-X (XRD) dan perubahan
morfologi pula diawasi menggunakan mikroskopi pengimbasan elektron pancaran
medan (FESEM). Perubahan komposisi nanotiub titania ditentukan dengan
penyerakan tenaga sinar-X (EDX). Kesan voltan penganodan, nisbah isipadu
elektrolit dan kandungan NH4F ke atas morfologi dan geometri nanotiub
titania telah dikaji. Sifat elektrolit mempengaruhi penertiban dan keseragaman
nanotiub. Tambahan pula, pelbagai diameter nanotiub berukuran dari 62 – 112 nm
dan 1.1 – 1.3 mm panjang dapat dicapai melalui
pengawalan voltan penganodan dan nisbah isipadu EG/Gly. Penganodan Ti pada 20V
dalam nisbah isipadu 1:1 EG/Gly yang mengandungi 0.25 – 1.0 wt.% NH4F
merupakan keadaan optimum dalam pengawalan penertiban nanotiub.
Kata kunci: titania, nanotiub,
penganodan gliserol, etilena glikol
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