Microwave Sintering of Nanocrystalline TiO2

1990 ◽  
Vol 189 ◽  
Author(s):  
J. A. Eastman ◽  
K. E. Sickafus ◽  
J. D. Katz ◽  
S. G. Boeke ◽  
R. D. Blake ◽  
...  

ABSTRACTNanocrystalline TiO2 compacts having initial approximate mean grain sizes of 14 nm and approximate green densities of 70% of theoretical were sintered by short-time exposure in a 2.45 GHz microwave cavity to maximum temperatures of 800, 1000 or 1200 ºC. Sample densities were measured before and after exposure to microwaves using Archimede's method. Transmission electron microscopy and x-ray diffraction were utilized to monitor grain growth and phase changes. Rutherford backscattering was used to monitor any changes in oxygen stoichiometry. The results of this study indicate that enhanced densification behavior is obtained for microwavesintered samples relative to samples sintered using conventional pressureless-sintering techniques.

2017 ◽  
Vol 13 (2) ◽  
pp. 4640-4647
Author(s):  
A. M. Abdelghany ◽  
M.S. Meikhail ◽  
S.I. Badr ◽  
A. S. Momen

Thin film samples of pristine polyvinyl chloride (PVC), poly vinyldine fluoride (PVDF) in combination with their blend in addition to samples containing factorial mass fraction of multi wall carbon nano-tubes (MWCNTs) in the dopant level were prepared via routine casting technique using tetrahydrofurane (THF) as a common solvent. X-ray diffraction and transmission electron microscopy (TEM) depict the nano-scale (15-25 nm) of functionalized MWCNTs with no surface damage results from functionalization process.X-ray diffraction (XRD) shows a semi-crystalline nature of PVDF with evidence for more than one phase namely a and b phases. The fraction of b phase was calculated and correlated to the dopant content. FTIR optical absorption spectra revels a preservation of the main vibrational bands before and after addition of MWCNTs in the doping level with a presence of new small band 1151 cm-1 assigned for the interaction and complexation between constituents.


2018 ◽  
Vol 12 (3) ◽  
pp. 240-247
Author(s):  
Anna Szczygielska ◽  
Zbigniew Pędzich ◽  
Wojciech Maziarz

This work describes the production of nanocrystalline TiO2 and SnO2 oxides, as well as their nanocomposites (containing 26.9, 58.7 and 79.0wt.% of SnO2) with two-stage sol-gel method combined with high temperature treatment. The phase composition and medium size crystallites were determined using X-ray diffraction analysis (XRD) and revealed that the nanocomposites crystallize in tetragonal structures of TiO2 - anatase and SnO2 - cassiterite. Specific surface area of the nanopowders, measured using sorption method (BET), changed from 42.1 to 160.8m2/g. The morphology of the nanopowders was observed using transmission electron microscope (TEM). As indicated by TEM images, the manufactured nanopowders were well crystallized and consisted of small, spherical grains. The obtained nanopowders were also tested for NH3 gas detection application. The presented method of nanopowders synthesis enables to obtain nanocrystalline TiO2 and SnO2 oxides, as well as composites from TiO2-SnO2 of known and controlled chemical and phase composition. It also enables to obtain composites used for gas sensors. The sensor made of composite containing 58.7wt.% of SnO2 exhibited the best NH3 sensing features.


2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Mashael Alshabanat ◽  
Amal Al-Arrash ◽  
Waffa Mekhamer

Polymer nanocomposites of polystyrene matrix containing 10% wt of organo-montmorillonite (organo-MMT) were prepared using the solution method with sonication times of 0.5, 1, 1.5, and 2 hours. Cetyltrimethylammonium bromide (CTAB) is used to modify the montmorillonite clay after saturating its surface with Na+ions. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were used to characterize the montmorillonite before and after modification by CTAB. The prepared nanocomposites were characterized using the same analysis methods. These results confirm the intercalation of PS in the interlamellar spaces of organo-MMT with a very small quantity of exfoliation of the silicate layers within the PS matrix of all samples at all studied times of sonication. The thermal stability of the nanocomposites was measured using thermogravimetric analysis (TGA). The results show clear improvement, and the effects of sonication time are noted.


2020 ◽  
Vol 2020 ◽  
pp. 1-10
Author(s):  
Thuy-Chinh Nguyen ◽  
Tien-Dung Nguyen ◽  
Duc-Toan Vu ◽  
Duc-Phuong Dinh ◽  
Anh-Hiep Nguyen ◽  
...  

This paper presents some characteristics, properties, and morphology of TiO2 nanoparticles (nano-TiO2) modified with various contents of 3-(trimethoxysilyl)propyl methacrylate (TMSPM) coupling agent. The treatment process was carried out in ethanol solvent at 50oC using ammonia as a catalyst for hydrolysis reaction of silane to silanol. Infrared spectroscopy, thermogravimetric analysis, transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, ultraviolet-visible spectroscopy, and X-ray diffraction methods were used for determination of the characteristics, properties of nano-TiO2 before and after treatment. In addition, the contact angle and grafting efficiency of TMSPM on the surface of TiO2 nanoparticles was also evaluated. The obtained results confirmed that TMSPM was grafted to the TiO2 nanoparticles, the agglomeration of nano-TiO2 was decreased, and surface of TiO2 nanoparticles became hydrophobic after modification by TMSPM.


Nanomaterials ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 64 ◽  
Author(s):  
L. Andrés Guerrero ◽  
Lenys Fernández ◽  
Gema González ◽  
Marjorie Montero-Jiménez ◽  
Rafael Uribe ◽  
...  

A hydrogen peroxide (H2O2) sensor and biosensor based on modified multi-walled carbon nanotubes (CNTs) with titanium dioxide (TiO2) nanostructures was designed and evaluated. The construction of the sensor was performed using a glassy carbon (GC) modified electrode with a TiO2–CNT film and Prussian blue (PB) as an electrocalatyzer. The same sensor was also employed as the basis for H2O2 biosensor construction through further modification with horseradish peroxidase (HRP) immobilized at the TiO2–fCNT film. Functionalized CNTs (fCNTs) and modified TiO2–fCNTs were characterized by Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR), and X-Ray DifFraction (XRD), confirming the presence of anatase over the fCNTs. Depending on the surface charge, a solvent which optimizes the CNT dispersion was selected: dimethyl formamide (DMF) for fCNTs and sodium dodecylsulfate (SDS) for TiO2–fCNTs. Calculated values for the electron transfer rate constant (ks) were 0.027 s−1 at the PB–fCNT/GC modified electrode and 4.7 × 10−4 s−1 at the PB–TiO2/fCNT/GC electrode, suggesting that, at the PB–TiO2/fCNT/GC modified electrode, the electronic transfer was improved. According to these results, the PB–fCNT/GC electrode exhibited better Detection Limit (LD) and Quantification Limit (LQ) than the PB–TiO2/fCNT/GC electrode for H2O2. However, the PB film was very unstable at the potentials used. Therefore, the PB–TiO2/fCNT/GC modified electrode was considered the best for H2O2 detection in terms of operability. Cyclic Voltammetry (CV) behaviors of the HRP–TiO2/fCNT/GC modified electrodes before and after the chronoamperometric test for H2O2, suggest the high stability of the enzymatic electrode. In comparison with other HRP/fCNT-based electrochemical biosensors previously described in the literature, the HRP–fCNTs/GC modified electrode did not show an electroanalytical response toward H2O2.


2008 ◽  
Vol 600-603 ◽  
pp. 239-242
Author(s):  
Ariadne Andreadou ◽  
Jörg Pezoldt ◽  
Christian Förster ◽  
Efstathios K. Polychroniadis ◽  
M. Voelskow ◽  
...  

One of the main challenging tasks in the prospective technology is the buckling suppression of the 3C-SiC film due to the melting and solidification process and the stress relief as a consequence of the short time Si melting during the Flash Lamp Annealing. To overcome this effect and to stabilize a flat surface morphology an alternative i-FlASiC process was developed. This work refers to the influence of the layer stack modifications by doping and meltstop formation by ion implantation on the wafer buckling. The samples were studied by transmission electron microscopy, high resolution x-ray diffraction and infrared ellipsometry. The aim was to optimize the doping and flash lamp annealing conditions in relation to the i-FLASiC layer stack modification.


1990 ◽  
Vol 213 ◽  
Author(s):  
Jeffrey A. West ◽  
James T. Manos ◽  
Michael J. Aziz

ABSTRACTThin films of Ni3Al formed by co-evaporation onto insulating substrates form a single phase fcc disordered lattice upon rapid solidification following excimer laserinduced melting with an interface velocity of ~4 m/s. Transmission Electron Microscopy (TEM) and x-ray diffraction (XRD) analyses exhibit no superlattice diffraction at room temperature. Resistivity measurements, indicating that the disordered phase has a higher resistivity and much smaller temperature coefficient at room temperature than the stable ordered (L12) phase, permit us to monitor phase changes and ordering on a fast time-scale. Subsequent annealing recovers long-range order, with resistivity measurements indicating that reordering begins just below 300°C.


2007 ◽  
Vol 336-338 ◽  
pp. 1270-1273 ◽  
Author(s):  
Wan Chang Sun ◽  
He Jun Li ◽  
Shou Yang Zhang ◽  
Yong Huang

The morphologies and textures of the pyrolytic carbon matrix in 2D-C/C composites after graphitization were investigated by means of polarized light microscope (PLM) and high resolution transmission electron microscope (HRTEM). The microstructure parameters of the pyrolytic carbon matrix before and after graphitization were characterized with X-ray diffraction (XRD) technology. It was found that the interplanar distance of (002) planes (d002) of pyrolytic carbon matrix decreases, and the microcrystalline stack height (LC) increases after graphitization. Graphitization treatment resulted in a coarsening of the surface texture and in the formation of circumferential cracks within the matrix. The lattice fringes of the pyrolytic carbon matrix are continuous and longer in each domain and the (002) peak spot is smaller and more intense after graphitization.


2008 ◽  
Vol 8 (12) ◽  
pp. 6445-6450
Author(s):  
F. Paraguay-Delgado ◽  
Y. Verde ◽  
E. Cizniega ◽  
J. A. Lumbreras ◽  
G. Alonso-Nuñez

The present study reports the synthesis method, microstructure characterization, and thermal stability of nanostructured porous mixed oxide (MoO3-WO3) at 550 and 900 °C of annealing. The material was synthesized using a hydrothermal method. The precursor was prepared by aqueous solution using ammonium heptamolibdate and ammonium metatungstate, with an atomic ratio of Mo/W = 1. The pH was adjusted to 5, and then the solution was transferred to a teflon-lined stainless steel autoclave and heated at 200 °C for 48 h. The resultant material was washed using deionized water. The specific surface area, morphology, composition, and microstructure before and after annealing were studied by N2 physisorption, scanning electron microscopy (SEM), analytical transmission electron microscopy (TEM), and X-Ray diffraction (XRD). The initial synthesized materials showed low crystallinity and high specific surface area around (141 m2/g). After thermal annealing the material showed higher crystallinity and diminished its specific surface area drastically.


2011 ◽  
Vol 391-392 ◽  
pp. 400-403
Author(s):  
Dong Mei Zhao ◽  
Li Guo Sun ◽  
Li Li Lv ◽  
Jian Li

Quasi-spherical gold nanoparticles(Au NPs) prepared by trisodium citrate reduction of HAuCl4were dispersed into cellulose acetate(CA) ultra-fine fibers by electrospinning. The optical properties of Au NPs before and after electrospinning were measured by UV-vis spectrometer. The morphology and distribution of Au NPs in CA ultra-fine fibers were observed by transmission electron microscopy (TEM). The morphology and diameter of Au NPs/CA fibers were studied by scanning electron microscopy (SEM). The crystallinity change of CA fiber before and after adding Au NPs was characterized by X-ray diffraction (XRD).


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