X-ray Powder Diffractometry. An Introduction. (Serie: Chemical Analysis, Vol. 138.) VonR. Jenkins undR. L. Snyder. John Wiley & Sons, New York, 1996. 391 S., geb. 87.95 £.—ISBN 0–471–51339–3

1997 ◽  
Vol 109 (12) ◽  
pp. 1417-1418 ◽  
Author(s):  
Robert J. Cernik
Keyword(s):  
New York ◽  
Author(s):  
G. H. Francis

SummaryConclusions concerning the unit-cell contents and chemical formula of a mineral are all too often drawn from a small part of the available data. A procedure is outlined by which any chemical analysis for which a density is available can be utilized, provided X-ray data are available for a reasonable range of analysed specimens. The effects of possible errors in the determination of water, and in the assessment of essential and non-exsential water, are discussed both qualitatively and quantitatively.A survey of all available data for anthophyllite has not disclosed any specimens in which the number of oxygen atoms per unit cell is significantly in excess of 96 with the possible exception of the Glen Urquhart gedrite and the Edwards (New York) material. But it is certain that the number of cations per unit cell is normally well in excess of 60 (partial occupation of the A lattice positions), and that, although ‘excess’ water in sonic fibrous anthophyllites may be adsorbed impurity, the number of hydroxyl groups in others is well in excess of 8 per unit cell; it is also fairly clear that the number of hydroxyl groups may fall below 8 per unit cell.


Author(s):  
R. Sinclair ◽  
B.E. Jacobson

INTRODUCTIONThe prospect of performing chemical analysis of thin specimens at any desired level of resolution is particularly appealing to the materials scientist. Commercial TEM-based systems are now available which virtually provide this capability. The purpose of this contribution is to illustrate its application to problems which would have been intractable until recently, pointing out some current limitations.X-RAY ANALYSISIn an attempt to fabricate superconducting materials with high critical currents and temperature, thin Nb3Sn films have been prepared by electron beam vapor deposition [1]. Fine-grain size material is desirable which may be achieved by codeposition with small amounts of Al2O3 . Figure 1 shows the STEM microstructure, with large (∽ 200 Å dia) voids present at the grain boundaries. Higher quality TEM micrographs (e.g. fig. 2) reveal the presence of small voids within the grains which are absent in pure Nb3Sn prepared under identical conditions. The X-ray spectrum from large (∽ lμ dia) or small (∽100 Ǻ dia) areas within the grains indicates only small amounts of A1 (fig.3).


Author(s):  
M. Vallet-Regí ◽  
M. Parras ◽  
J.M. González-Calbet ◽  
J.C. Grenier

BaFeO3-y compositions (0.35<y<0.50) have been investigated by means of electron diffraction and microscopy to resolve contradictory results from powder X-ray diffraction data.The samples were obtained by annealing BaFeO2.56 for 48 h. in the temperature range from 980°C to 1050°C . Total iron and barium in the samples were determined using chemical analysis and gravimetric methods, respectively.In the BaFeO3-y system, according to the electron diffraction and microscopy results, the nonstoichiometry is accommodated in different ways as a function of the composition (y):In the domain between BaFeO2.5+δBaFeO2.54, compositional variations are accommodated through the formation of microdomains. Fig. la shows the ED pattern of the BaFeO2.52 material along thezone axis. The corresponding electron micrograph is seen in Fig. 1b. Several domains corresponding to the monoclinic BaFeO2.50 phase, intergrow with domains of the orthorhombic phase. According to that, the ED pattern of Fig. 1a, can be interpreted as formed by the superposition of three types of diffraction maxima : Very strong spots corresponding to a cubic perovskite, a set of maxima due to the superposition of three domains of the monoclinic phase along [100]m and a series of maxima corresponding to three domains corresponding to the orthorhombic phase along the [100]o.


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