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.

scholarly journals Synthesis and characterization of sol-gel derived monophasic mullite powder

Cerâmica ◽  
2020 ◽  
Vol 66 (379) ◽  
pp. 307-313
Author(s):  
A. Jana ◽  
D. Ray
Keyword(s):  
Sol Gel ◽  
Grain Morphology ◽  
Precursor Powder ◽  
Bet Surface Area ◽  
X Ray Diffraction ◽  
Heating Rates ◽  
X Ray ◽  
Heat Treated ◽  
Different Temperatures

Abstract High-purity microfine mullite precursor powder of stoichiometric chemical composition, 3Al2O3.2SiO2, was synthesized through the sol-gel route using aluminum isopropoxide and tetraethyl orthosilicate. The derived mullite precursor powder was characterized by BET surface area, particle size distribution, Fourier-transform infrared spectroscopy, thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy. Phase analysis of the precursor powder and calcined samples at different temperatures was done by XRD. Non-isothermal crystallization kinetics of mullite precursor was studied by TG-DTA in static air using heating rates of 5.0, 7.5, 10.0, 12.5, and 15 K.min-1. Grain morphology was studied by SEM. The results showed that synthesized mullite precursor powder possessed homogeneity of Al and Si components, and the amorphous precursor powder was converted to monophasic mullite crystal when heat-treated at 970 °C. Based on Flynn-Wall-Ozawa and Kissinger equations, the activation energy associated with the crystallization of mullite was determined to be 1189.8 and 1189.0 kJ.mol-1, respectively.

scholarly journals Morphology of Thin Film Composite Membranes Explored by Small-Angle Neutron Scattering and Positron-Annihilation Lifetime Spectroscopy

Membranes ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 48 ◽  
Author(s):  
Vitaliy Pipich ◽  
Marcel Dickmann ◽  
Henrich Frielinghaus ◽  
Roni Kasher ◽  
Christoph Hugenschmidt ◽  
...  
Keyword(s):  
Thin Film ◽  
Neutron Scattering ◽  
Positron Annihilation ◽  
Small Angle ◽  
Small Angle Neutron Scattering ◽  
Positron Annihilation Lifetime Spectroscopy ◽  
Film Composite ◽  
Positron Annihilation Lifetime ◽  
Thin Film Composite

The morphology of thin film composite (TFC) membranes used in reverse osmosis (RO) and nanofiltration (NF) water treatment was explored with small-angle neutron scattering (SANS) and positron-annihilation lifetime spectroscopy (PALS). The combination of both methods allowed the characterization of the bulk porous structure from a few Å to µm in radius. PALS shows pores of ~4.5 Å average radius in a surface layer of about 4 μm thickness, which become ~40% smaller at the free surface of the membranes. This observation may correlate with the glass state of the involved polymer. Pores of similar size appear in SANS as closely packed pores of ~6 Å radius distributed with an average distance of ~30 Å. The main effort of SANS was the characterization of the morphology of the porous polysulfone support layer as well as the fibers of the nonwoven fabric layer. Contrast variation using the media H2O/D2O and supercritical CO2 and CD4 identified the polymers of the support layers as well as internal heterogeneities.

scholarly journals Synthesis and Characterization of Co-Mo/γ-Alumina Catalyst from local Kaolin clay for Hydrodesulfurization of Iraqi Naphtha

2021 ◽  
Vol 11 (1) ◽  
pp. 84-106
Author(s):  
Nada Sadoon Ahmed zeki ◽  
Sattar Jalil Hussein ◽  
Khalifa K. Aoyed ◽  
Saad Kareem Ibrahim ◽  
Ibtissam K. Mehawee
Keyword(s):  
Surface Area ◽  
Sulfur Removal ◽  
Sulfuric Acid Concentration ◽  
Bet Surface Area ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mo Catalyst ◽  
Pressure Time ◽  
Al2o3 Catalyst

This work deals with the hydrodesulfurization of three types of naphtha feedstocks; mixednaphtha (WN), heavy naphtha (HN) & light naphtha (LN) with a sulfur content of 1642.1,1334.9 & 709 ppm respectively, obtained from Missan refinery using prepared Co-Mo/γ-Al2O3catalyst. The Iraqi white kaolin was used as a starting material for the preparation of γ-Al2O3support, transferring kaolin to meta-kaolin was studied through calcination at differenttemperatures and durations, kaolin structure was investigated using X-Ray diffractiontechniques.High purity 94.83%. Crystalline γ-Al2O3 with a surface area of 129.91 m2/gm, pore volume0.9002 cm3/g was synthesized by extraction of Iraqi kaolin with H2SO4 at different acid to clayweight ratios, acid concentrations & leaching time. Ethanol was used as precipitating agent; theresultant gel was dried and calcined at 70OC, 10 hrs & 900 OC, 2 hrs respectively.The effects of different parameters on the average crystallinity and extraction % ofsynthesized γ-Al2O3 were studied like; acid: clay ratio, sulfuric acid concentration, leachingtime, leaching temperature & kaolin conversion to metakaolin. Characterization of prepared γ-Al2O3 & Co-Mo catalyst were achieved by X-ray diffraction, FTIR-spectra, texture properties& BET surface area, BJH N2 adsorption porosity, AFM, SEM, crush strength & XRF tests. Co-Mo/ γ-Al2O3 catalyst with final loading 5.702 wt% and 21.45 wt% of Co and Mo oxidesrespectively was prepared by impregnation methods.The activity of prepared Co-Mo/γ-Al2O3 catalyst after moulding to be tested forhydrodesulfurization (HDS) of naphtha feedstock W.N, H.N & L.N was performed using apilot hydrotreating unit at petroleum research & development centre, at different operatingconditions. Effects of temperature, LHSV, pressure, time & pore size distribution were studied,the best percentage of sulfur removal is increased with decreasing LHSV to 2 hr-1 as a generaltrend to be 89.71, 99.72, 99.20 % at 310oC for the whole naphtha, heavy naphtha and lightnaphtha feedstocks respectively, at 34 bar pressure and 200/200 cm3/cm3 H2/HC ratio.

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 Preparation and Characterization of Rh/MgSNTs Catalyst for Hydroformylation of Vinyl Acetate: The Rh0 was Obtained by Calcination

Catalysts ◽  
2019 ◽  
Vol 9 (3) ◽  
pp. 215 ◽  
Author(s):  
Penghe Su ◽  
Ya Chen ◽  
Xiaotong Liu ◽  
Hongyuan Chuai ◽  
Hongchi Liu ◽  
...  
Keyword(s):  
Vinyl Acetate ◽  
Atomic Emission ◽  
Catalytic Performance ◽  
Bet Surface Area ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Atomic Emission Spectrometer ◽  
Calcination Method

A simple and practical Rh-catalyzed hydroformylation of vinyl acetate has been synthesized via impregnation-calcination method using silicate nanotubes (MgSNTs) as the supporter. The Rh0 (zero valent state of rhodium) was obtained by calcination. The influence of calcination temperature on catalytic performance of the catalysts was investigated in detail. The catalysts were characterized in detail by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectrometer (XPS), atomic emission spectrometer (ICP), and Brunauer–Emmett–Teller (BET) surface-area analyzers. The Rh/MgSNTs(a2) catalyst shows excellent catalytic activity, selectivity and superior cyclicity. The catalyst could be easily recovered by phase separation and was used up to four times.

Fabrication and Characterization of TiO2 Nanotubes for Dye-Sensitized Solar Cells

2015 ◽  
Vol 1131 ◽  
pp. 215-220
Author(s):  
Emmanuel Nyambod Timah ◽  
Buagun Samran ◽  
Udom Tipparach
Keyword(s):  
Solar Cells ◽  
Anatase Phase ◽  
Dye Sensitized Solar Cells ◽  
Ammonium Fluoride ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dye Sensitized ◽  
Dc Power ◽  
Sensitized Solar Cells

TiO2nanotubes were successfully synthesized by anodization method of Ti foils. The electrolyte was composed of ethylene glycol (EG), ammonium fluoride (0.3%wt NH4F) and de-ionized water (2% vol H2O). A constant DC power supply of 50 V was used during anodization with anodizing times of 1 hour, 2 hours, 4 hours and 6 hours. The samples were annealed at 450 °C for 2 hours. The TiO2nanotubes were studied by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). Structural analysis revealed the presence of pure Ti, and the crystalline anatase phase due to transformation of amorphous TiO2after annealing. The morphology of TiO2nanotube sizes showed an increase in tube diameter with anodizing time from approximately 50 nm to 200 nm. However, the efficiency of dye-sensitized solar cells increased with anodizing times up to a maximum of 5.74 % for anodizing time of 4 hours.

Microstructure Characterization of the Reaction Interface between CBN Grain and Titanium-Deposited Film

2012 ◽  
Vol 538-541 ◽  
pp. 166-171
Author(s):  
Wen Feng Ding ◽  
Yang Min Liang ◽  
Jian He ◽  
Li Tang ◽  
Jie Yu ◽  
...  
Keyword(s):  
Heating Temperature ◽  
Cubic Boron Nitride ◽  
High Vacuum ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
X Ray ◽  
Energy Dispersion Spectrometer ◽  
Heat Treated ◽  
Deposited Film

Cubic boron nitride (CBN) abrasive grains with surface titanium-deposited film were heat-treated during 550-950°C for 60 min under high vacuum circumstance. Detailed interfacial compounds analysis by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion spectrometer (EDS), differential thermal analysis (DTA) indicates that the interfacial reactions are much dependent on the heating temperature to some extents, and the reaction products, TiN, TiB2 and TiB chiefly form the network structure. In particular, at 950°C the transition layers with excellent performance, CBN/TiB2/TiB/(TiB+TiN)/TiN/CBN, is realized.

Preparation, Characterization of Nonmetal Doped TiO2 Nanoparticles with their Excellent Photocatalystic Properties

2011 ◽  
Vol 183-185 ◽  
pp. 2254-2257
Author(s):  
Ying Wei Wang ◽  
Yu Fei Li ◽  
Pei Han Yang
Keyword(s):  
Photoelectron Spectroscopy ◽  
Photocatalytic Performance ◽  
Anatase Phase ◽  
Titania Nanoparticles ◽  
X Ray Diffraction ◽  
X Ray ◽  
One Step ◽  
Doped Titania ◽  
Nonmetal Doping

Nonmetal (S, P) doped titania nanoparticles were synthesized by a one step hydrothermal method. These samples were calcined with different temperature, the sample exist in anatase phase has much higher photocatalytic activity for methylene blue (MB) degradation. The visible response and the higher UV activity of the different nonmetal doped TiO2make it possible to utilize solar energy efficiently to execute photocatalysis processes. The resulting materials were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), etc. It can conclude the nonmetal doping TiO2proves to be more suitable to improve the photocatalytic performance.

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