scholarly journals Solid Acids from Persulphated and Perchlorated Physical Mixtures of Zirconium and Titanium Hydroxides

2002 ◽  
Vol 20 (10) ◽  
pp. 977-993
Author(s):  
Gamal M.S. El Shafei ◽  
Christine A. Philip
Keyword(s):  
Tetragonal Phase ◽  
Anatase Phase ◽  
Nitrogen Adsorption ◽  
Rutile Phase ◽  
Acid Sites ◽  
Solid Acids ◽  
Monoclinic Zirconia ◽  
Anion Adsorption ◽  
Physical Mixtures ◽  
Structural Aspects

Calcination at 650°C of a physical mixture of zirconium and titanium hydroxides led to the formation of the corresponding oxides, monoclinic zirconia and anatase. The adsorption of perchlorate or persulphate anions (as 0.05, 0.1, 0.2 or 0.4 M aqueous solutions) before calcination did not inhibit crystallization; however, perchlorate anions activated the formation of rutile in addition to the predominant anatase phase. Indeed, the adsorption of perchlorated anions prior to calcination allowed the thermodynamically less stable tetragonal phase of zirconia to be detected in addition to monoclinic zirconia at ambient temperature. In contrast, the adsorption of persulphate anions before calcination stabilized the tetragonal phase with no rutile phase being detected in this case. Infrared spectroscopy showed that adsorbed S2O82– anions were held more strongly by the solid than ClO4− anions which tended to decompose when the solid was calcined. The acidities of the solid acids produced because of S2O82– or ClO4−anion adsorption were studied via the adsorption of pyridine (pKa = 5.3) from cyclohexane solution. The amounts and strengths of the acid sites formed during persulphate treatment were higher than those resulting from perchlorate adsorption. The strength of the acid sites formed on samples calcined before loading with S2O82– or ClO4− anions showed no significant differences. Variations detected in the structural aspects arising from S2O82– or ClO4− anion adsorption were reflected in the texture as assessed by nitrogen adsorption at −196°C.

scholarly journals Preparation and High-Throughput Testing of TiO2-Supported Co Catalysts for Fischer‒Tropsch Synthesis

Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 352
Author(s):  
Christian Schulz ◽  
Peter Kolb ◽  
Dennis Krupp ◽  
Lars Ritter ◽  
Alfred Haas ◽  
...  
Keyword(s):  
High Throughput ◽  
Anatase Phase ◽  
Rutile Phase ◽  
Tropsch Synthesis ◽  
Performance Tests ◽  
Fischer Tropsch ◽  
Fischer Tropsch Synthesis ◽  
Co Catalysts ◽  
Impregnation Technique ◽  
Co Conversion

A series of Co/TiO2 catalysts was tested in a parameters field study for Fischer‒Tropsch synthesis (FTS). All catalysts were prepared by the conventional impregnation technique to obtain an industrially relevant Co content of 10 wt % or 20 wt %, respectively. In summary, 10 different TiO2 of pure anatase phase, pure rutile phase, as well as mixed rutile and anatase phase were used as supports. Performance tests were conducted with a 32-fold high-throughput setup for accelerated catalyst benchmarking; thus, 48 experiments were completed within five weeks in a relevant operation parameters field (170 °C to 233.5 °C, H2/CO ratio 1 to 2.5, and 20 bar(g)). The most promising catalyst showed a CH4 selectivity of 5.3% at a relevant CO conversion of 60% and a C5+ productivity of 2.1 gC5+/(gCo h) at 207.5 °C. These TiO2-based materials were clearly differentiated with respect to the application as supports in Co-catalyzed FTS catalysis. The most prospective candidates are available for further FTS optimization at a commercial scale.

scholarly journals Unexpected Link between the Template Purification Solvent and the Structure of Titanium Dioxide Hollow Spheres

Catalysts ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 112
Author(s):  
Tamás Gyulavári ◽  
Kata Kovács ◽  
Klára Magyari ◽  
Kornélia Baán ◽  
Anna Szabó ◽  
...  
Keyword(s):  
Titanium Dioxide ◽  
Photocatalytic Activity ◽  
Phase Composition ◽  
Anatase Phase ◽  
Hollow Spheres ◽  
Rutile Phase ◽  
Carbon Sphere ◽  
Carbon Spheres ◽  
Carbonate Species ◽  
Determining Factor

Carbon spheres were applied as templates to synthesize titanium dioxide hollow spheres. The templates were purified with either ethanol or acetone, and the effects of this treatment on the properties of the resulting titania were investigated. The photocatalytic activity of the catalysts was measured via the decomposition of phenol model pollutant under visible light irradiation. It was found that the solvent used for the purification of the carbon spheres had a surprisingly large impact on the crystal phase composition, morphology, and photocatalytic activity. Using ethanol resulted in a predominantly rutile phase titanium dioxide with regular morphology and higher photocatalytic activity (r0,phenol = 3.9 × 10−9 M∙s−1) than that containing mainly anatase phase prepared using acetone (r0,phenol = 1.2 × 10−9 M∙s−1), surpassing the photocatalytic activity of all investigated references. Based on infrared spectroscopy measurements, it was found that the carbon sphere templates had different surface properties that could result in the appearance of carbonate species in the titania lattice. The presence or absence of these species was found to be the determining factor in the development of the titania’s properties.

In Situ High-Temperature Transmission Electron Microscopy Observations of the Formation of Nanocrystalline TiC from Nanocrystalline Anatase (TiO2)

1998 ◽  
Vol 4 (3) ◽  
pp. 269-277 ◽  
Author(s):  
A. Agrawal ◽  
J. Cizeron ◽  
V.L. Colvin
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Temperature ◽  
Solid Phase ◽  
Anatase Phase ◽  
High Resolution Electron Microscopy ◽  
Rutile Phase ◽  
Transmission Electron ◽  
New Phase

In this work, the high-temperature behavior of nanocrystalline TiO2 is studied using in situ transmission electron microscopy (TEM). These nanoparticles are made using wet chemical techniques that generate the anatase phase of TiO2 with average grain sizes of 6 nm. X-ray diffraction studies of nanophase TiO2 indicate the material undergoes a solid-solid phase transformation to the stable rutile phase between 600° and 900°C. This phase transition is not observed in the TEM samples, which remain anatase up to temperatures as high as 1000°C. Above 1000°C, nanoparticles become mobile on the amorphous carbon grid and by 1300°C, all anatase diffraction is lost and larger (50 nm) single crystals of a new phase are present. This new phase is identified as TiC both from high-resolution electron microscopy after heat treatment and electron diffraction collected during in situ heating experiments. Video images of the particle motion in situ show the nanoparticles diffusing and interacting with the underlying grid material as the reaction from TiO2 to TiC proceeds.

scholarly journals Fabrication, N-doping Mechanism and Evaluation of N-doped TiO2 Thin Films Based on Laser Ablation Method

2009 ◽  
Vol 2 (1) ◽  
pp. 17-23 ◽  
Author(s):  
S. Somekawa ◽  
Y. Kusumoto ◽  
H. Yang ◽  
M. Abdulla-Al-Mamun ◽  
B. Ahmmad
Keyword(s):  
Crystal Structure ◽  
Methylene Blue ◽  
Photocatalytic Activity ◽  
Laser Ablation ◽  
Anatase Phase ◽  
Rutile Phase ◽  
Laser Ablation Method ◽  
Dye Decomposition ◽  
N Doping ◽  
Keywords Laser

The relation among the change of the crystal structure, the amount of doped N and the photocatalytic activity for the decomposition of methylene blue was studied. The N-doping was promoted by the change of the crystal structure from the rutile phase to the anatase phase. The photocatalytic activity for the decomposition of methylene blue was enhanced by an increase in the amount of anatase crystals and doped N. Keywords: Laser ablation; N-doping process; Crystal change; N-doped TiO2 thin film; Dye decomposition. © 2010 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved. DOI: 10.3329/jsr.v2i1.2992        J. Sci. Res. 2 (1), 17-23 (2010) 

Probing the Phase Transition in Nanocrystalline TiO2 Powders by Positron Lifetime (PAL) Technique

2011 ◽  
Vol 319-320 ◽  
pp. 151-159 ◽  
Author(s):  
E.M. Hassan ◽  
Basma A.A. Balboul ◽  
M.A. Abdel-Rahman
Keyword(s):  
Positron Annihilation ◽  
Anatase Phase ◽  
Rutile Phase ◽  
Bet Surface Area ◽  
X Ray Diffraction ◽  
Positron Annihilation Lifetime ◽  
Nanocrystallite Size ◽  
Heat Treated ◽  
Degussa P25

Positron annihilation techniques (PAT) have recently been successfully employed for the characterization of phase transitions in metals and compounds. In the present study, positron annihilation lifetime (PAL) measurements have been carried out on a nanocrystalline titania (TiO2) in the form of powders that had been heat-treated at temperatures ranging from 300 to 1273K. The PAL spectra were analyzed into two lifetime components. The shorter lifetime τ1 (185-300 ps) is attributed to positron annihilation in vacancies and the longer lifetime τ1 (400-580 ps) to positrons in microviods at interfaces. The rutile phase of TiO2 powders was utilized as a reference in order to compare their behavior with the commercially supplied and widely available anatase phase (Degussa P25). The influence of the heat-treatment upon the nanostructure during the transition of the anatase to rutile phase were also investigated by X-ray diffraction (XRD), TEM and BET surface area methods. Understanding of this effect is expected to enhance our knowledge of the morphology and nanocrystallite size of TiO2 powders and their T-dependence, and hence their physical properties.

Synthesis of Titania coated Alumina Particles by a Hybrid Sol-gel Method

2002 ◽  
Vol 740 ◽  
Author(s):  
A.D. Schmidt ◽  
S.B. Majumder ◽  
P.S. Dobal ◽  
R.S. Katiyar ◽  
D.C. Agrawal
Keyword(s):  
Anatase Phase ◽  
Sol Gel ◽  
Rutile Phase ◽  
Microscopy Imaging ◽  
Nano Crystalline ◽  
Heat Treated ◽  
Alumina Particles ◽  
Gel Technique ◽  
Titania Coatings ◽  
Titania Coating

ABSTRACTModifying their surface with a coating of another ceramic material can dramatically alter the properties of ceramic particles. In the present work we have demonstrated that the Al2O3 particles can be successfully coated by TiO2 using a novel sol-gel technique. The nature of these coatings was predicted on the basis of scanning electron microscopy imaging in conjunction with the micro-Raman scattering measurements. The surface morphology of these particles shows that either individual or group of sub-micron alumina particles are coated with the nano-crystalline titania particles. The thickness of the titania coating could be varied by changing the precursor sol concentration. Amorphous titania was converted to anatase phase at 400°C and upon further heating it started transforming to rutile phase, and both these phases coexisted in the coated particles that were heat treated up to 800°C. The mechanical strength of the titania coating was measured qualitatively by ultrasonicating the coated powders for longer duration to observe that titania coatings are strongly adhered with the alumina particles.

scholarly journals Hydrothermal Synthesis of rGO-TiO2 Composites as High-Performance UV Photocatalysts for Ethylparaben Degradation

Catalysts ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 520 ◽  
Author(s):  
Miller Ruidíaz-Martínez ◽  
Miguel A. Álvarez ◽  
María Victoria López-Ramón ◽  
Guillermo Cruz-Quesada ◽  
José Rivera-Utrilla ◽  
...  
Keyword(s):  
High Performance ◽  
Photocatalytic Performance ◽  
Raw Materials ◽  
Anatase Phase ◽  
Titanium Isopropoxide ◽  
Rutile Phase ◽  
Pure Tio2 ◽  
New Materials ◽  
Reduced Graphene ◽  
Structural Surface

A series of reduced graphene oxide-TiO2 composites (rGO-TiO2) were prepared by hydrothermal treatment using graphite and titanium isopropoxide as raw materials. The structural, surface, electronic, and optical properties of the prepared composites were extensively characterized by N2 adsorption, FTIR, XRD, XPS, Raman spectroscopy, and DRS. GO was found to be effectively reduced and TiO2 to be in pure anatase phase in all composites obtained. Finally, experiments were performed to evaluate the effectiveness of these new materials as photocatalysts in the degradation of ethylparaben (EtP) by UV radiation. According to the band-gap energies obtained (ranging between 3.09 eV for 4% rGO-TiO2 to 2.55 eV for 30% rGO-TiO2), the rGO-TiO2 composites behave as semiconductor materials. The photocatalytic activity is highest with a rGO content of 7 wt% (7% rGO-TiO2), being higher than observed for pure TiO2 (Eg = 3.20 eV) and achieving 98.6% EtP degradation after only 40 min of treatment. However, the degradation yield decreases with higher percentages of rGO. Comparison with rGO-P25 composites showed that a better photocatalytic performance in EtP degradation is obtained with synthesized TiO2 (rGO-TiO2), probably due to the presence of the rutile phase (14.1 wt %) in commercial P25.

Optical and Electrical Properties of TiO2 Nanotubes Grown by Titanium Anodization

2009 ◽  
Vol 1178 ◽  
Author(s):  
Yahya Alivov ◽  
Vladimir Kuryatkov ◽  
Mahesh Pandikunta ◽  
Gautam Rajanna ◽  
Daniel Johnstone ◽  
...  
Keyword(s):  
Optical Properties ◽  
Electrical Properties ◽  
Tio2 Nanotubes ◽  
Anatase Phase ◽  
Rutile Phase ◽  
Electrochemical Anodization ◽  
Voltage Range ◽  
Wide Range ◽  
Transient Spectroscopy ◽  
Tio2 Nts

AbstractIn this work we investigated the structural, electrical, and optical properties of titanium dioxide (TiO2) nanotubes (NTs) formed by electrochemical anodization of Ti metal sheets in NH4F+glycerol electrolyte at different anodization voltages (Va) and acid concentrations. Our results revealed that TiO2 NTs can be grown in a wide range of anodization voltages from 10 V to 240 V. The maximum NH4F acid concentration, at which NTs can be formed, decreases with the anodization voltage, which is 0.7% for Va<60V, and decreases to 0.1% at Va =240 V. Glancing angle X-ray diffraction (GAXRD) experiments show that as-grown amorphous TiO2 transforms to anatase phase after annealing at 400 oC, and further transforms to rutile phase at annealing temperatures above 500 oC. Samples grown in 30-120 voltage range have higher crystal quality as seen from anatase (101) peak intensity and reduced linewidth. The electrical resistivity of the NTs varies with Va concentration and increases by eight orders of magnitude when Va increases from 10 V to 240 V. This is consistent with cathodoluminescense studies which showed improved optical properties for samples grown in this voltage range. Optical properties of samples were also studied by low temperature photoluminescence. Temperature dependent I-V and photo-induced current transient spectroscopy were employed to analyze electrical properties and defect structure on NT samples.

Growth of TiO2 Nanotube Arrays using Porous Anodic Alumina Templates

2013 ◽  
Vol 1601 ◽  
Author(s):  
A. Shoja ◽  
A. Nourmohammadi ◽  
M. H. Feiz
Keyword(s):  
Anatase Phase ◽  
Sol Gel ◽  
Rutile Phase ◽  
Nanotube Arrays ◽  
Nanoporous Alumina ◽  
Heat Treated ◽  
Semiconductor Behavior ◽  
Dc Electric Field ◽  
Nanoporous Alumina Templates ◽  
Anodic Alumina Templates

ABSTRACTThe aim of this research study is to produce high quality TiO2 nanotube arrays. It is shown that sol-gel electrophoresis is a suitable one to obtain vast-area TiO2 nanotube arrays when nanoporous alumina templates are used. To fabricate TiO2 nanotube arrays, alumina templates were produced via a two-step anodizing by a homemade anodizing cell using high purity phosphoric acid as the electrolyte with aluminum and platinum as electrodes. The semiconductor behavior of these templates can also be employed when producing conducting substrates for the grown TiO2 nanotubes. Stabilized titanium sol was prepared by modified hydrolysis of the titanium precursor using acetic acid. In order to produce TiO2 nanotube arrays, the template pores were filled with the precursor sol by applying a DC electric field. Then, the filled template was heat treated to crystallize the desired TiO2 phase. Scanning electron microscopy of TiO2 nanotube arrays showed that the nanotubes have been deposited in the channels of the nanoporous alumina template. X-ray diffraction data confirmed phase structure and composition of TiO2 nanotube arrays after heat treatment. To reach pure anatase phase, the samples were heated at 320°C and 400°C for two hours. To obtain pure rutile phase, the samples were heated at 320°C and 750°C for two hours.

Effect of Iron and Vanadium on the Phase Transition of Titanium Dioxide Obtained by Polymeric Precursor Method

2016 ◽  
Vol 881 ◽  
pp. 18-23
Author(s):  
Eduardo Felipe de Carli ◽  
Maycon dos Santos ◽  
Natali Amarante da Cruz ◽  
Daniela Cristina Manfroi ◽  
Jusinei Meireles Stropa ◽  
...  
Keyword(s):  
Phase Transition ◽  
Titanium Dioxide ◽  
Phase Formation ◽  
Anatase Phase ◽  
Synthesis Method ◽  
Rutile Phase ◽  
Polymeric Precursor Method ◽  
Polymeric Precursor ◽  
Precursor Method ◽  
Powder Samples

The titanium dioxide phase formation is dependent on the synthesis method, temperature of calcination and modifiers insertion. By using chemical methods, such as Polymeric Precursor Method, the organic impurities or extrinsic defects caused by doping play an important rule on the formation of precursor structure before the phase crystallization above 500 oC. Some dopants can change the decomposition mechanism of the precursor, which affects the anatase-rutile phase transition. In this work, the Polymeric Precursor Method was used to synthesize titanium dioxide powder samples in order to investigate the effects of iron (III) and vanadium (V) dopants on the phase formation. Through thermal analysis of polymeric precursors and X-ray diffractometry for calcined powder samples it was possible to show the existence of antagonistic effects for both investigated dopants. While the iron doping reduces the anatase phase tetragonality and delays the rutile phase conversion, the vanadium one changes the mechanism of decomposition of polymeric precursor and leads to more amount of rutile phase.

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