Malaysian Journal of Analytical Sciences, Vol 20 No 2 (2016): 373 - 381 373 MALAYSIAN JOURNAL OF ANALYTICAL SCIENCES Published by The Malaysian Analytical Sciences Society 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 Chin 1 *, Zulkarnain Zainal 2, 3 , Zuraida Khusaimi 1 , Siti Sarah Ismail 1 1 School of Chemistry and Environment, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia 2 Department of Chemistry, Faculty of Science 3 Advanced 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 NH 4 F 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.% NH 4 F 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 NH 4 F 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 m 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.% NH 4 F merupakan keadaan optimum dalam pengawalan penertiban nanotiub. Kata kunci: titania, nanotiub, penganodan gliserol, etilena glikol ISSN 1394 - 2506