The co- and cross-polarized scattered intensity ratios for 3D layered structures with randomly rough interfaces

Cliff and Lorimer (1) have proposed a simple approach to thin foil x-ray analy sis based on the ratio of x-ray peak intensities. However, there are several experimental pitfalls which must be recognized in obtaining the desired x-ray intensities. Undesirable x-ray induced fluorescence of the specimen can result from various mechanisms and leads to x-ray intensities not characteristic of electron excitation and further results in incorrect intensity ratios.In measuring the x-ray intensity ratio for NiAl as a function of foil thickness, Zaluzec and Fraser (2) found the ratio was not constant for thicknesses where absorption could be neglected. They demonstrated that this effect originated from x-ray induced fluorescence by blocking the beam with lead foil. The primary x-rays arise in the illumination system and result in varying intensity ratios and a finite x-ray spectrum even when the specimen is not intercepting the electron beam, an ‘in-hole’ spectrum. We have developed a second technique for detecting x-ray induced fluorescence based on the magnitude of the ‘in-hole’ spectrum with different filament emission currents and condenser apertures.

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Valence state analysis of elements by EPMA and its application

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100134752 ◽

1990 ◽

Vol 48 (2) ◽

pp. 230-231

Author(s):

Chen Liqing ◽

Liu Zuqin ◽

Zhang Wei

Keyword(s):

Valence State ◽

Line Intensities ◽

Valence States ◽

Valence Electrons ◽

Fe And Mn ◽

Intensity Ratios ◽

State Analysis

Valence state analyses of Fe and Mn in oxides by EPMA have been reported in literature. In this paper, the effects of valence state on intensity ratios ILα/IKα and ILα/ILβ of Cu, Ni, Co, Fe, Mn, Cr and their oxides, and on intensity ratios ILβ2/ILα1 and ILγ1/ILα1 of Mo, Nb, Zr and their oxides were studied. It was observed that intensity ratios change with valence states in accordance with some regularities, and these effects could be utilized for analyzing the valence states of catalysts.Valence state analysis of elements by EPMA is based on the fact that changes in the states of valence electrons in the outer shells of an atom cause corresponding changes in line intensities. The M electrons of Cu, Ni, Co, Fe, Mn, Cr and the N electrons of Mo, Nb, Zr are valence electrons. Line Kα1,2 and six lines of L are produced from the transitions of K-L2,3 and L-M or L-N respectively.

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Electron diffraction studies of amorphous and polycrystalline thin films

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100173728 ◽

1990 ◽

Vol 48 (4) ◽

pp. 118-119

Author(s):

D J H Cockayne ◽

D R McKenzie

Keyword(s):

Thin Films ◽

Electron Diffraction ◽

Polycrystalline Materials ◽

Good Resolution ◽

Scattered Intensity ◽

Radial Density ◽

X Ray ◽

Polycrystalline Thin Films ◽

Nitrogen Ion ◽

Diffraction Patterns

The study of amorphous and polycrystalline materials by obtaining radial density functions G(r) from X-ray or neutron diffraction patterns is a well-developed technique. We have developed a method for carrying out the same technique using electron diffraction in a standard TEM. It has the advantage that studies can be made of thin films, and on regions of specimen too small for X-ray and neutron studies. As well, it can be used to obtain nearest neighbour distances and coordination numbers from the same region of specimen from which HREM, EDS and EELS data is obtained.The reduction of the scattered intensity I(s) (s = 2sinθ/λ ) to the radial density function, G(r), assumes single and elastic scattering. For good resolution in r, data must be collected to high s. Previous work in this field includes pioneering experiments by Grigson and by Graczyk and Moss. In our work, the electron diffraction pattern from an amorphous or polycrystalline thin film is scanned across the entrance aperture to a PEELS fitted to a conventional TEM, using a ramp applied to the post specimen scan coils. The elastically scattered intensity I(s) is obtained by selecting the elastically scattered electrons with the PEELS, and collecting directly into the MCA. Figure 1 shows examples of I(s) collected from two thin ZrN films, one polycrystalline and one amorphous, prepared by evaporation while under nitrogen ion bombardment.

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