Structural, Optical and Magnetic Properties of Nanocrystalline Cobalt Doped TiO2 Prepared by Sol-Gel Route

2013 ◽  
Vol 24 ◽  
pp. 168-175
Author(s):  
Kirit S. Siddhapara ◽  
D.V. Shah

Nanocrystalline Cobalt-doped TiO2was prepared by Sol-Gel technique, followed by freeze-drying treatment at-30°C temperature for 12hrs. The obtained Gel was thermally treated at 200,400,600, 800°C. 1%, 2% and 4% Cobalt doped TiO2nanopowder has been prepared X-ray Powder Diffraction (XRD), Scanning Electron microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDX), was used to study its structural properties. The XRD pattern shows the coexistence of anatase phase and rutile phase. Thermal gravimetric analysis shows Cobalt concentration affects thermal decomposition. UV-Vis Spectroscopy, Photo luminescence (PL), was used to study its Optical properties. Optical Bandgap were calculated with the incorporation of different concentration of cobalt. UV-Visible spectroscopy show variation in band gap for the sample treated at different temperature for same concentration. All Cobalt doped TiO2nanostructures shows an appearance of Red shift relative to the bulk TiO2. The determination of magnetic properties was also carried out by Vibrating Sample Magnetometer.

2013 ◽  
Vol 665 ◽  
pp. 118-126
Author(s):  
Kirit S. Siddhapara ◽  
D.V. Shah

Nanocrystalline Fe-doped TiO2 was prepared by Sol-Gel technique, which was followed by freeze at-30°C temperature for 12hrs. The obtained Gel was thermally treated at 200,400,600 and 800°C. X-ray Powder Diffraction (XRD), Scanning Electron microscopy (SEM), UV-Vis Spectroscopy, Photo luminescence (PL) and EDAX was used to study its Structural and Optical properties. All Fe-doped TiO2 nanostructures show an appearance of Red shift relative to the bulk TiO2. The XRD pattern show the coexistence of major anatase phase and minor brookite phase for samples treated up to 600°C. Whereas at 800°C rutile is the only phase observed. All Fe doped TiO2 nanostructures show an appearance of Red shift relative to bulk undoped TiO2. The magnetic property by Gouy Balance of Fe doped TiO2 exhibit Peramagnetism at room temperature.


2018 ◽  
Vol 930 ◽  
pp. 73-78
Author(s):  
Eduardo Felipe de Carli ◽  
Natali Amarante da Cruz ◽  
Hiana Muniz Garcia ◽  
Jusinei Meireles Stropa ◽  
Lis Regiane Vizolli Favarin ◽  
...  

Important changes in anatase crystal structure are responsible for the consequent anatase-to-rutile phase transition in titanium dioxide powders. In order to investigate several structural rearrangements occurring in anatase phase obtained by hydrolysis-based method such as Sol-Gel method the X-ray diffraction techniques followed by Rietveld method seems to better approach. Several alterations in anatase lattice parameters can occur by doping insertion and the investigation of isostructural zircon silicate can provide interesting ones. In the present paper, the monitoring of anatase structure reordering and the consequent anatase-to-rutile phase transition along the thermal treatment up to higher temperatures were monitored carrying out DSC and XRD characterizations. The insertion of 6 mol% of zircon silicate leads to the fully anatase stabilization up to 900 °C due the control of ordering process, even that a continuous increasing in anatase tetragonality is present during the entire process. We can conclude the reconstructive anatase-to-rutile phase transition is delayed to very higher temperatures can consequence of more stable cross-linked metal oxide bond in anatase phase.


2019 ◽  
Vol 56 ◽  
pp. 28-38 ◽  
Author(s):  
Uraiwan Werapun ◽  
Jaraslak Pechwang

TiO2 and iron-doped TiO2 were synthesized by sol-gel method. TiO2 and 0.5 %mol Fe:TiO2 were calcined at 500 and 800 °C for 3 h. The synthesized particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), UV-VIS diffuse reflectance spectrophotometry (UV/DRS), scanning electron microscopy (SEM) and scanning electron microscope-energy dispersive X-Ray analysis (SEM-EDX). The XRD patterns of all samples that were calcined at 500 °C showed only anatase phase. On increasing temperature from 500 to 800 °C, the anatase phase transformed to rutile phase. For 0.5 %mol Fe:TiO2, pseudobrookite (Fe2TiO5) phase was observed at 800 °C. The particles that contained rutile showed higher antibacterial activities against E.coli, B. subtilis, and S. aureus than anatase phase, under fluorescent irradiation.


1997 ◽  
Vol 12 (2) ◽  
pp. 439-443 ◽  
Author(s):  
R. Rodríguez-Talavera ◽  
S. Vargas ◽  
R. Arroyo-Murillo ◽  
R. Montiel-Campos ◽  
E. Haro-Poniatowski

Titania matrices prepared by a sol-gel technique were doped with several cations (La, Zn, Al, K, Na, Ca, Ba, and Co). The effect of the dopants on the thermal and structural properties of the materials is analyzed. The dopant concentration was 2% mol with respect to titanium, and in all cases the same anion (nitrate) was used. The transition temperatures from amorphous to anatase and from anatase to rutile were measured using x-ray diffraction. The amorphous-anatase transition is independent, for almost all samples, of the type of dopant used; however, the anatase-to-rutile phase transition depends strongly on the kind of cation. This means that the temperature range where the anatase phase exists can be controlled by choosing the appropriate dopant. We have found a correlation between the anatase-rutile phase transition temperature and the radius of the cations and their electric charge.


2014 ◽  
Vol 896 ◽  
pp. 481-484 ◽  
Author(s):  
Nafi'ah Ardhani ◽  
Agus Supriyanto ◽  
Akhmad Herman Yuwono ◽  
Risa Suryana

TiO2 nanoparticles have been successfully synthesized using the sol-gel method with main materials of titanium tetraisopropoxide (TTIP) and HClO4 solutions. Mass ratios (Rw) of aquadest and TTIP were 0.85, 2.00, and 3.50 which were going to be investigated in crystallization of TiO2 phases. Pre-heating was performed on TiO2 at 60°C for one day then it was annealed at 150°C for 3 hours. The DSSC structure was formed by using the synthesized-TiO2 as semiconductor material and beta-carotene as dye sensitizer. The x-ray diffraction (XRD) spectrum indicated that TiO2 peaks had anatase phases on crystal orientation of (101), (004), and (200) while TiO2 of rutile phase only appeared on orientation of (211). The highest intensity for all Rw was dominated by (101) anatase phase. From XRD spectrum data of (101) peak, the Scherrer’s method predicted that crystal size of TiO2 was 3.48 nm, 4.36 nm, and 4.47 nm for Rw of 0.85, 2.00, and 3.50, respectively. The Tauc’s method was applied on the UV-Vis data that predicted the bandgap energy (Eg) of TiO2 for Rw of 2.00 (Eg=3.14 eV) was higher than Rw of 0.85 (Eg=3.02 eV) and 3.50 (Eg=3.04 eV). The I-V characteristic calculation of DSSC structures were obtained that the efficiency optimum is 0.01% for Rw of 2.00. It is considered that bandgap energy value correlated to stability of Ti-OH bonds that caused the exited-electrons are easily injected to conduction band of TiO2. The performance of DSSC using the synthesized-TiO2 which consists of anatase and rutile can be improved about ten times compared to that using the pure-TiO2 rutile.


2021 ◽  
Vol 16 (4) ◽  
pp. 804-815
Author(s):  
Candra Purnawan ◽  
Sayekti Wahyuningsih ◽  
Oktaviani Nur Aniza ◽  
Octaria Priwidya Sari

TiO2 and TiO2 doped Cd, Co, Mn (TiO2-M) were synthesized with a sol-gel method, and the photocatalytic activity of Remazol Brilliant Blue R and Remazol Yellow FG has been conducted. TiO2-M (Cd, Co, Mn) was synthesized with the mol Ti:M ratio of 3:1, and the materials were calcined at 300, 400, and 500 °C. The materials were characterized by X-ray Diffraction (XRD), Scanning Electron Microscopy-Energy Dispersive X-ray (SEM-EDX), and UV-Vis Reflectance. The XRD result shows that at the temperature of 300 °C TiO2 and TiO2-M formed tend to be amorphous. At 400 °C the anatase phase is formed, while at 500 °C the rutile phase begins to form. And overall, the crystallinity of TiO2 is higher than metal-doped TiO2. The UV-Vis Reflectance result showed that the bandgap energy of all doping materials (TiO2-M) decreased. The larger the metal ion radius of dopant, the larger the crystal size obtained  and then the higher the bandgap obtained. The results of SEM-EDX showed that the morphology of TiO2 was spherical and regular, whereas the morphology of TiO2-M had a smoother surface due to the influence of metal doping. Photocatalytic activity of TiO2-M on Remazol Brilliant Blue R and Remazol Yellow FG was greater than TiO2. The optimum pH of the solution was obtained at pH 5 and the optimum catalyst phase was obtained at the anatase phase. The percentages degradation for 30 min of Remazol Brilliant Blue R were 67.34% (TiO2), 92.12% (TiO2-Co), 85.47% (TiO2-Mn), and 83.91% (TiO2-Cd), while for Remazol Yellow FG they were 58.84% (TiO2), 74.61% (TiO2-Co), 67.93% (TiO2-Mn) and 64.19% (TiO2-Cd), respectively. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0). 


2015 ◽  
Vol 93 (1) ◽  
pp. 106-112 ◽  
Author(s):  
Lijia Liu ◽  
Jun Li ◽  
Tsun-Kong Sham

Freestanding TiO2 nanograss–nanotube hierarchical membranes are synthesized from a Ti metal foil by electrochemical anodization. It is found that the two nanostructures exhibit different luminescence properties, which are also affected by the crystal phases upon phase transformation. An unusual near-UV luminescence is observed from the amorphous nanograss, which is found to be excitation element specific. The amorphous nanotube shows no luminescence. Upon calcination, both nanograss and nanotubes are crystalized into the anatase phase with some rutile phase present, and both structures emit visible green luminescence at slightly different energies. The luminescence mechanism is explored using UV–vis spectroscopy, X-ray absorption near-edge structures (XANES), and X-ray excited optical luminescence (XEOL), and its implications are presented.


2011 ◽  
Vol 1352 ◽  
Author(s):  
Varun Chaudhary ◽  
Amit K. Srivastava ◽  
Jitendra Kumar

ABSTRACTTiO2 nanoparticles have been prepared by sol-gel process using titanium isopropoxide as a precursor with ethanol and water as solvents. The synthesis involves gel formation, digestion for 24h, drying at 100oC for 10h, and calcination in air at 500-800oC for 2h. The resulting powder has been studied with respect to phase(s), morphology, optical absorption and photo -luminescence (PL) behaviour. The calcination of dried sol-gel product at 500oC for 2h leads to formation of anatase phase that possesses a tetragonal structure (a = 3.785 Å, c = 9.514 Å, Z = 4), average crystallite size ~ 11 nm and band gap of 3.34 eV. Further, increasing the time (t) of calcination causes crystallite growth that follows the relation d = α – β exp (-t/τ), α = 18.1 nm, β = 9.6 nm and τ = 6.9h. However, calcination of sol-gel product at 800oC for 2h gives rise to a rutile phase (tetragonal a = 4.593Å, c = 2.959Å, Z = 2), average crystallite size ~ 25 nm and band gap of 3.02 eV. The anatase phase exhibits strong PL emission peaks (excitation wavelength 405 nm) at 2.06 and 1.99 eV due to defect levels within the energy band gap. This observation has been attributed to finite size effects occurring in nanoparticles.


2013 ◽  
Vol 800 ◽  
pp. 464-470 ◽  
Author(s):  
Wei Chao Liu ◽  
Huan Yan Xu ◽  
Tian Nuo Shi ◽  
Li Cheng Wu ◽  
Ping Li

TiO2/tourmaline composite photocatalyst was prepared by sol-gel method using tetrabutyl orthotitanate (Ti (OC4H9)4) as a precursor. As a comparison, pure TiO2 was prepared at the same experimental conditons without the addition of tourmaline. The obtained composite photocatalyst was characterized by X-Ray diffraction (XRD) and scanning electron microscope (SEM) and its photocatalytic activity was also investigated through the photodiscoloration of methyl orange (MO) under UV irradiation. The XRD results indicated that, in the composite photocatalyst, TiO2 existed in the form of anatase and rutile, with the sintering temperature and tourmaline content increasing, the anatase phase trended to the transformation to rutile phase. The SEM results revealed that the nanosized particles of TiO2 were well dispersed and immobilized on the surface of tourmaline, especially for the sample with 2% tourmaline content. Compared with pure TiO2, the composite photocatalyst exhibited a higher photocatalytic activity. When the pure TiO2 was used as the photocatalyst, the MO discoloration ratio only reached 55%. However, the MO discoloration ratio could approach 100% in presence of TiO2/tourmaline composit photocatalyst under the same conditions. The effects of tourmaline content and sintering temperature on the photocatalytic activity of the composite were studied in this work and the results suggested that the sample with 2% tourmaline content and sintered at the temperature of 550°C exhibited the best photocatalytic activity. Finally, the possible mechanism for the photodiscoloration of MO was put forward.


2008 ◽  
Vol 8 (5) ◽  
pp. 2410-2418 ◽  
Author(s):  
A. Ahmad ◽  
S. Buzby ◽  
C. Ni ◽  
S. Ismat Shah

Nb and Sc doped TiO2 nanoparticles were synthesized via sol–gel technique. Dopant concentration of each element was varied from 0.5 to 1.5 atomic%. The effect of metal ion doping and calcination temperatures on anatase to rutile phase transformation has been investigated. Samples were analyzed by various analytical methods such as X-ray diffraction (XRD), Transmission Electron Microscope (TEM), X-ray Photoelectron Spectroscopy (XPS) and Energy Dispersive X-ray Spectroscopy (EDS). XRD analyses showed that Nb and Sc doped samples calcined at 300 °C and 350 °C, respectively, were crystalline and had an anatase structure. Results showed that anatase was stable up to 700 °C annealing temperature for samples doped with 0.5 atomic% Nb. There was a sharp transition from anatase to rutile phase above 700 °C and complete rutile structure was obtained at 750 °C. However, the transformation from anatase to rutile was not so sharp in samples doped with 1.0 atomic% and 1.5 atomic% Nb. Results indicated that higher concentration of Nb helps to stabilize the anatase phase. For samples doped with 0.5 atomic% Sc, anatase phase is stable up to 650 °C. Transformation from anatase to rutile starts at temperature above 650 °C and 100% rutile phase was obtained at 800 °C while for samples doped with 1.0 atomic% and 1.5 atomic% Sc, the complete transformation from anatase to rutile takes place at an even higher temperature. Results indicate that increasing the calcination time from 0.5 to 2.0 hours at 500 °C does not affect the stability of anatase phase. However, TEM and XRD data showed that the increase in the annealing time leads to an increase in particles size. The rutile to anatase concentration ratio increased with temperature above the phase transformation temperature. The activation energy for the phase transformation from anatase to rutile for doped and undoped samples was also measured. There was a general rise in the activation energy with increasing dopant concentration.


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