Effect of Fluoride Concentration and Water Content on Morphology of Titania Nanotubes in Ethylene Glycol Solution

2013 ◽  
Vol 829 ◽  
pp. 907-911 ◽  
Author(s):  
Meysam Naghizadeh ◽  
Saber Ghannadi ◽  
Hossein Abdizadeh ◽  
Mohammad Reza Golobostanfard
Keyword(s):  
Ethylene Glycol ◽  
Water Content ◽  
Fluoride Concentration ◽  
Pure Titanium ◽  
Ammonium Fluoride ◽  
Electrochemical Anodization ◽  
Nanotube Arrays ◽  
Geometrical Parameters ◽  
High Concentration ◽  
Inner Diameter

Titanium dioxide (TiO2) nanotube arrays were prepared at room temperature by electrochemical anodization of a pure titanium foil in electrolyte solutions containing ethylene glycol as a solvent and de-ionized water and ammonium fluoride as additives. Since the morphology and size of TiO2 nanotubes play critical roles in determining their performance, the control of geometrical parameters of the nanotube arrays including length and inner diameter are of great importance. The present research demonstrates the significant effects of fluoride concentration and water content in anodizing electrolyte on formation of nanotubes and their dimensions. Scanning electron microscope investigation shows that nanotube arrays are no longer formed in very low or very high concentration of ammonium fluoride. Also, increase in fluoride concentration causes increase in lengths and inner diameters of the nanotubes. Moreover, it is evident that the maximum nanotube growth rate was achieved in medium amount of water. In addition, it is found that the nanotube inner diameter increases by adding more water to the solution.

scholarly journals Electrochemical Anodization and Characterization of Titanium Oxide Nanotubes for Photo Electrochemical Cells

2021 ◽  
Vol 2070 (1) ◽  
pp. 012073
Author(s):  
C U Bhadra ◽  
D Henry Raja ◽  
D Jonas Davidson
Keyword(s):  
Titanium Oxide ◽  
Oxygen Vacancies ◽  
Ammonium Fluoride ◽  
Band Gap Energy ◽  
Electrochemical Anodization ◽  
Nanotube Arrays ◽  
Photoluminescence Intensity ◽  
Titania Nanotube Arrays ◽  
Titanium Oxide Nanotubes ◽  
Inner Diameter

Abstract Due to its multitude of applications, titanium oxide is one of the most coveted and most sought-after materials. The above experiment demonstrated that TiO2 nanotube arrays might be formed by electrochemical anodization of titanium foil. The 0.25 wt% ammonium fluoride (NH4F) was added to a solution of 99% ethylene glycol. Anodization is carried out at a constant DC voltage of 12V for 1 hour. Then, the annealing process is carried out for 1 hour at 4800C, which is known as an annealing. FE-SEM were utilized to evaluate the surface morphology of the nanotube arrays that were made. At the wavelength of 405 nm, sharply peaked photoluminescence intensity was observed, which corresponded tothe band gap energy (3.2 eV) of the anatase TiO2 phase. Since free excitations appear at 391 and 496 nm, and since oxygen vacancies are developed on the surface of titania nanotube arrays, it is reasonable to conclude that free excitations and oxygen vacancies are the causes of humps at 391 and 496 nm, and that they may also be present at 412 and 450 nm. FESEM results showed uniformly aligned TiO2 nanotube arrays with an inner diameter of 100 nm and a wall thickness of 50 nm

C-axis preferentially oriented and fully activated TiO2 nanotube arrays for lithium ion batteries and supercapacitors

2014 ◽  
Vol 2 (29) ◽  
pp. 11454-11464 ◽  
Author(s):  
Dengyu Pan ◽  
He Huang ◽  
Xueyuan Wang ◽  
Liang Wang ◽  
Haobo Liao ◽  
...  
Keyword(s):  
Titanium Dioxide ◽  
Ethylene Glycol ◽  
Lithium Ion Batteries ◽  
Oxygen Vacancies ◽  
Lithium Ion ◽  
Tio2 Nanotube Arrays ◽  
Nanotube Arrays ◽  
High Concentration ◽  
Oxygen Conditions ◽  
Titanium Dioxide Nanotube Arrays

We report the fabrication of long titanium dioxide nanotube arrays with highly c-axis preferentially oriented crystallization and a high concentration of oxygen vacancies by second anodization in ethylene glycol and annealing under poor-oxygen conditions.

scholarly journals Study the Effect of Water Content on the Structure of Electrochemically Prepared TiO2 Nanotubes

2022 ◽  
Author(s):  
Sara Al-Waisawy ◽  
Ahmed Kareem Abdullah ◽  
Hadi A. Hamed ◽  
Ali A. Al-bakri
Keyword(s):  
Water Content ◽  
Pure Titanium ◽  
Electrochemical Anodization ◽  
X Ray Diffraction ◽  
Force Microscopy ◽  
Atomic Force ◽  
Titania Nanotube Arrays ◽  
Anodization Process ◽  
Titania Films ◽  
Average Size

In this research, the pure titanium foil was treated in glycerol base electrolyte with 0.7 wt.% NH4F and a small amount of H2O at 17 V for 2 hours by electrochemical anodization process in order to prepare Titania nanotube arrays at room temperature (~25 ºC), different water content was added to the electrolyte as a tube enhancing agent. The high density uniform arrays are prepared by using organized and well aligned these tubes. The average size of tube diameter, ranging from 57 to 92 nm which found it increases with increasing water content, and the length of the tube ranging from 2.76 to 4.12 µm, also found to increase with increasing water content and ranging in size of wall thickness from 23 to 35 nm. A possible growth mechanism is presented. The X-ray diffraction (XRD), atomic force microscopy (AFM), and scanning electron microscopy (SEM) were utilized to study the structure and morphology of the Titania films.

The Effect of Preparation Temperature of Electrolytes on Undoped and Ag-Doped TiO2 Nanotube Structures

2016 ◽  
Vol 860 ◽  
pp. 7-11 ◽  
Author(s):  
Somkuan Photharin ◽  
Buagun Samran ◽  
Rinnatha Vongwatthaporn ◽  
Narongsak Kodtharin ◽  
Ramida Chaiyarat ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Electrolyte Solution ◽  
Pure Titanium ◽  
Silver Ions ◽  
Ammonium Fluoride ◽  
Electrolyte Solutions ◽  
Nanotube Arrays ◽  
X Ray Diffraction ◽  
Preparation Temperature ◽  
X Ray

In this work, we present the effect of preparation temperature of electrolytes for fabricating undoped and silver (Ag) doped titanium dioxide (TiO2) nanotubes by the electrochemical anodic oxidation of pure titanium sheets in electrolytes, mixtures of ethylene glycol (EG), ammonium fluoride (NH4F) and deionized water, that contain with different of silver ions. Heat treatment of electrolytes was carried out at 100 °C during preparation process. The morphology and structure of prepared nanotubes were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The structures of TiO2 nanotubes obtained from heat treatment and non-heat treatment of electrolyte solutions and adding silver ions in electrolyte solution are similar. The nanotubes appear in arrays and the diameters of nanotubes were about 92 nm for non-heat treatment electrolyte solution and undoped TiO2 and about 102 nm for heat treatment electrolyte solution and all Ag-doped TiO2 nanotube arrays. When the concentration of silver nitrate (AgNO3) increases, the TiO2 nanotube arrays cracked and are not well arranged.

SELF-ORDERING ELECTROCHEMICAL SYNTHESIS OF TiO2 NANOTUBE ARRAYS: CONTROLLING THE NANOTUBE GEOMETRY AND THE GROWTH RATE

2011 ◽  
Vol 10 (01n02) ◽  
pp. 55-58 ◽  
Author(s):  
KRISHNA KANT ◽  
DUSAN LOSIC
Keyword(s):  
Growth Rate ◽  
Ethylene Glycol ◽  
Electrochemical Synthesis ◽  
The Self ◽  
Electrochemical Anodization ◽  
Nanotube Arrays ◽  
Anodization Voltage ◽  
Nanotube Array ◽  
Anodization Time ◽  
Nanotube Growth

We report the fabrication of highly ordered TiO 2 nanotube arrays employing electrochemical anodization of titanium using an organic electrolyte comprised of water, NH 4 F , and ethylene glycol. To achieve the self-ordering regime of TiO 2 nanotube growth and reliable fabrication optimal potential window between 80 and 100 V was determined. We show that anodization voltage can be used not only to control nanotube diameters (70–180 nm) but also to have impact on nanotube growth rate. The anodization voltage and anodization time were used to adjust the length of TiO 2 nanotube (thickness of nanotube layer). TiO 2 nanotube array films and self-supporting layers with thickness from < 5 μm to > 250 μm were routinely fabricated.

scholarly journals Fabrication of TiO2 Nanotube by Electrochemical Anodization: Toward Photocatalytic Application

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
O. Zakir ◽  
R. Idouhli ◽  
M. Elyaagoubi ◽  
M. Khadiri ◽  
A. Aityoub ◽  
...  
Keyword(s):  
Tio2 Nanotubes ◽  
Pure Titanium ◽  
Size Control ◽  
Ammonium Fluoride ◽  
Electrode System ◽  
Electrochemical Anodization ◽  
Voltage Range ◽  
X Ray ◽  
Self Organized ◽  
Type Semiconductor

In this study, a self-organized nanotubular titanium dioxide (TiO2) array was successfully produced by anodizing pure titanium in a mixture of glycerol, distilled water (8% vol.), and ammonium fluoride using a dual electrode system. The size control and distribution of the nanopores were performed in a DC voltage range varying from 30 V to 60 V. The diameter of TiO2 nanopores varies from 59 to 128 nm depending on the anodizing voltage. Energy-dispersive X-ray spectroscopy (EDX) analysis reveals that the as-prepared films are essentially composed of TiO2. According to the X-ray diffraction (XRD) and Raman spectroscopy analysis, the nanotubular arrays of TiO2 annealed at 600°C for 2 hours are composed of a phase mixture of anatase and rutile. Mott-Schottky analysis showed that the TiO2 nanotubes are consistent with an n-type semiconductor with a donor density of about 1017 cm-3. Preliminary results on the photocatalytic degradation of a pharmaceutical pollutant showed that the TiO2 nanotubes can be used as a promising material for application in wastewater treatment.

EFFECT OF VOLTAGE ON TIO2 NANOTUBES FORMATION IN ETHYLENE GLYCOL SOLUTION

2017 ◽  
Vol 79 (5-2) ◽  
Author(s):  
Syahriza Ismail ◽  
Khairil Azwa Khairul ◽  
Nurul Asyikin Ahmad Nor Hisham ◽  
Md Shuhazlly Mamat ◽  
Mohd Asyadi Azam
Keyword(s):  
Heat Treatment ◽  
Ethylene Glycol ◽  
Crystalline Phase ◽  
Tio2 Nanotubes ◽  
Oxygen Vacancies ◽  
Ammonium Fluoride ◽  
Nanotube Arrays ◽  
Anodization Voltage ◽  
Ionic Mobilities ◽  
Glycol Solution

The crystalline phase of the TiO2 nanotubes without further heat treatment were studied. The TiO2 nanotube arrays were produced by anodization of Ti foil at three different voltage; 10, 40, and 60 V in a bath with electrolytes composed of ethylene glycol (EG), ammonium fluoride (NH4F), and hydrogen peroxide (H2O2). The H2O2 is a strong oxidizing agent which was used as oxygen provider to increase the oxidation rate for synthesizing highly ordered and smooth TiO2 nanotubes. Anodization at voltage greater than 10 V leads to the formation of tubular structure where higher anodization voltage (~ 60 V) yield to larger tube diameter (~ 180 nm). Crystallinity of the nanotubes is improved as the voltage was increased. The transformation of amorphous to anatase can be obtained for as anodized TiO2 without any heat treatment. The Raman spectra results show the anodization at 40 V and 60 V gives anatase peak in which confirms the crystalline phase. The stabilization of the crystalline phase is due to the oxygen vacancies and ionic mobilities during the anodization at high voltage. 

Effect of Water Content on Structural and Photoelectrochemical Properties of Titania Nanotube Synthesized in Fluoride Ethylene Glycol Electrolyte

2012 ◽  
Vol 501 ◽  
pp. 204-208 ◽  
Author(s):  
Yingchin Lim ◽  
Zulkarnain Zainal ◽  
Mohd Zobir Hussein ◽  
Weetee Tan
Keyword(s):  
Ethylene Glycol ◽  
Water Content ◽  
Dimensional Change ◽  
Electrochemical Anodization ◽  
X Ray Diffraction ◽  
Linear Sweep ◽  
X Ray ◽  
Effect Of Water ◽  
Lower Water Content ◽  
Scanning Electron

In this work, the effect of water content from < 1 to 100 vol% on the electrochemical anodization of titanium in ethylene glycol-based electrolyte was investigated. The samples were characterized using X-ray diffraction (XRD) and their dimensional change was monitored by field emission scanning electron microscopy (FE-SEM). It was found that the microstructure and morphology of TiO2 varies dramatically with the water content. Nanotubes become less ordered with increasing water content up to 50 vol%. At 75 vol% water, only porous structure could be observed. Most importantly, at fixed applied voltage, smoother but relatively longer tubes can be grown with lower water content. Varying water content has no effect on the crystalline phase of the resulted nanotubes. However, the intensity of anatase (101) peak increases with increasing water content, indicating better crystallinity of samples. Nanotubes obtained in 50 vol% water exhibit the highest photoresponse when tested using linear sweep photovoltammetry due to enhanced microstructure and crystallinity.

Synthesis of Self-Aligned Titanium Oxide Nanotube Arrays in Ammonium Fluoride-Ethylene Glycol Electrolytes with Different Water Contents

2012 ◽  
Vol 463-464 ◽  
pp. 788-792
Author(s):  
Sasitorn Thongyoy ◽  
Areeya Aeimbhu
Keyword(s):  
Electron Microscopy ◽  
Ethylene Glycol ◽  
Room Temperature ◽  
Titanium Substrate ◽  
Ammonium Fluoride ◽  
Nanotube Arrays ◽  
Water Based ◽  
Water Contents ◽  
Anodisation Process ◽  
Scanning Electron

The aim of this research is to fabricate of TiO2nanotube arrays by potentiostatic anodisation process on titanium sheets. Anodisation is carried out under various applied potentials ranging from 20 to 30 volts for 1-3 hours at room temperature. Anodised were conducted in 1-4 wt% NH4F, water-based electrolyte and ethylene glycol-based electrolyte. The morphology of the anodised surfaces were characterised by scanning electron microscopy. When titanium sheets were anodised in various conditions, surface morphology of anodised titanium change remarkably with the changing of applied voltages, chemical composition of the electrolyte and anodisation time. The results of the present work show that the highly ordered and uniformly distributed TiO2nanotubes on titanium substrate can be fabricated by using mixtures of NH4F, ethylene glycol and water with appropriate conditions. Moreover, the anodisation potential and the water content play significant roles in the formation of TiO2nanotube with different inner tube diameters. The length of TiO2nanotube was controlled by anodisation time.

Synthesis of Highly Ordered Nanotubular Oxide Layers on Ti-6Al-4V Alloys by Anodization Technique

2011 ◽  
Vol 219-220 ◽  
pp. 1541-1544
Author(s):  
Shi Kai Liu ◽  
Hong Sen Zuo ◽  
Hai Bin Yang ◽  
Wen Jun Zou ◽  
Zheng Xin Li
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Applied Voltage ◽  
Electrochemical Anodization ◽  
Tube Length ◽  
Nanotube Arrays ◽  
Anodization Time ◽  
Tc4 Alloy ◽  
Inner Diameter ◽  
Scanning Electron

Highly ordered nanotube arrays were fabricated via electrochemical anodization of Ti-6Al-4V (TC4) alloy foils in aqueous fluorine containing electrolytes. The formation of ordered nanotubular films was affected by the applied anodization potential and the anodization time. The optimal applied voltage and anodization time were 20V and 1h, respectively, as-prepared anodic nanotubular films were in highly ordered with the average inner diameter of about 120nm, the wall thickness of 17nm and the tube length about 300nm. The tubular nanostructures were examined by field emission scanning electron microscopy. The possible nanotube formation mechanism was also discussed.

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