Electron optical studies of the formation of vanadium pentoxide catalyst

Author(s):  
A. Legrouri

The oxides of vanadium, especially vanadium pentoxide, have been extensively studied because of their interesting physical properties particularly in catalysis. Vanadium pentoxide is generally used in the oxidation and ammoxidation of hydrocarbons.This catalyst has been prepared via the thermal decomposition of ammonium metavanadate (AMV) in air. Thermogravimetric analysis (TGA), infrared spectroscopy (IRS) and x-ray diffraction (XRD) techniques together with high resolution electron microscopy (HREM) and scanning electron microscopy (SEM) have enabled us to elucidate the physicochemical changes occurring during the decomposition process.According to TGA results, the decomposition of AMV commences at 150°C and is complete by 320°C leading to vanadium pentoxide by loss of ammonia and water with the formation of two intermediate compounds, namely at 190°C, ammonium bivanadate: (NH4)2V4 O11, and at 230°C, ammonium hexavanadate AHV: (NH4)2V6O16 . Samples for structural correlation studies were prepared by heating AMV in a stream of air for 2 hours at selected temperatures of 140, 190, 230, 320 and 400°C.

1995 ◽  
Vol 398 ◽  
Author(s):  
A. Tomasi ◽  
E. Galvanetto ◽  
F.C. Matacotta ◽  
P. Nozar ◽  
P. Scardi ◽  
...  

ABSTRACTA systematic study on phase formation and stabilisation in the Ba-Cu-C-O system in the temperature range 20-500°C, under various atmospheres, by traditional thermal analysis techniques, high temperature X-ray diffraction and high resolution electron microscopy, has permitted to identify and characterise the formation kinetics of a new copper containing phase isomorphic to γ-BaCO3.


1997 ◽  
Vol 3 (S2) ◽  
pp. 441-442
Author(s):  
P.A. Crozier ◽  
I.Y. Chan ◽  
C.Y. Chen ◽  
L.W. Finger ◽  
R.C. Medrud ◽  
...  

Low-dose high resolution electron microscopy (HREM) is a useful technique for elucidating the structure of zeolites. In recent years a number of zeolite structures have been solved using combinations of different characterization techniques including adsorption measurements, powder x-ray diffraction and low-dose high resolution electron microscopy (for example see ref. 2). We have used these techniques to study the structure of a novel zeolite material. However, great care must be exercised when interpreting data from these techniques in terms of crystal structural units. In this particular case, the structure was recently determined using single crystal x-ray diffraction and showed some surprises.Details of the synthesis of this zeolite are given elsewhere. The high adsorption capacity suggested that this zeolite possessed two interpenetrating channels (either a 10 and a 12 ring or two 12 ring channels). X-ray powder diffraction showed the material to be monoclinic with a= 18.5Å, b= 13.4 Å, c= 7.6 Å β = 101.5°).


Author(s):  
Jillian F. Banfield ◽  
David R. Veblen ◽  
David J. Smith

A new, naturally occurring polymorph of TiO2 has been identified. This mineral forms lamellae generally only a few nanometers wide in anatase from two localities near Bintal Valais, Switzerland. The abundance of this mineral in anatase is too low to allow investigation by X-ray diffraction. The unit cell determined by electron diffraction is triclinic, with a = 0.754 nm, b = 0.448 nm, c = 0.616 nm, α = 78.90°, β = 124.55°, γ = 96.54°. The coherently intergrown lamellae are oriented with b parallel to a of anatase; the interface is parallel to (103) anatase.


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