Intensity specimen

Figure 1. Device for controlled irradiation of polymer films—rotating plate with specimens (a), source (b)9 ventilator (c), and electronics for controlling of light intensity, specimens temperature, and rate of rotations, (d)...

Interplanar Spacings. Diffractometer alignment procedures require the use of a well-prepared polycrystalline specimen. Two standard samples found to be suitable are silicon and a-quartz (including Novaculite). The 26 values of several of the most intense reflections for these materials are listed in Table 7.6 (Tables of Interplanar Spacings d vs. Diffraction Angle 26 for Selected Targets, Picker Nuclear, White Plains, N.Y., 1966). To convert to d for Ka or to d for Ka2, multiply the tabulated d value (Table 7.6) for Ka by the factor given below ... 

The contrast for specimen detail in the field of view is gready enhanced by darkfield illumination (10). The degree of contrast and sensitivity of detection of smaH-object details depend on the relative indices of the specimen and the mounting Hquid and on the intensity of the illumination. Darkfield illumination is not, however, a satisfactory solution for biologists who need direct transmitted light in order to observe specimens, especially stained specimens. It is, however, very usefiil in detecting asbestos fibrils that often exist in door tiles or water and air samples as 20-nm fibers (10 times finer than the resolution of an asbestos analyst s usual microscope) (11). Darkfield illumination yields an uimatural appearance and difficulties in interpretation hence, a need for better contrast methods stiU exists. 

RESEARCH OF DEPENDENCE OF INTENSITY OF X-RAY RADIATION FROM PHYSICAL AND CHEMICAL PROPERTIES OF THIN-FILM SPECIMENS... 

At X-ray fluorescence analysis (XRF) of samples of the limited weight is perspective to prepare for specimens as polymeric films on a basis of methylcellulose [1]. By the example of definition of heavy metals in film specimens have studied dependence of intensity of X-ray radiation from their chemical compound, surface density (P ) and the size (D) particles of the powder introduced to polymer. Have theoretically established, that the basic source of an error of results XRF is dependence of intensity (F) analytical lines of determined elements from a specimen. Thus the best account of variations P provides a method of the internal standard at change P from 2 up to 6 mg/sm the coefficient of variation describing an error of definition Mo, Zn, Cu, Co, Fe and Mn in a method of the direct external standard, reaches 40 %, and at use of a method of the internal standard (an element of comparison Ga) value does not exceed 2,2 %. Experiment within the limits of a casual error (V changes from 2,9 up to 7,4 %) has confirmed theoretical conclusions. 

Fig. 2-22 Effect of stress intensity range dJC on crack propagation for a notched specimen of X60 steel in 3.5% NaCl solution at 0.1 Hz.

In X-Ray Fluorescence (XRF), an X-ray beam is used to irradiate a specimen, and the emitted fluorescent X rays are analyzed with a crystal spectrometer and scintillation or proportional counter. The fluorescent radiation normally is diffracted by a crystal at different angles to separate the X-ray wavelengths and therefore to identify the elements concentrations are determined from the peak intensities. For thin films XRF intensity-composition-thickness equations derived from first principles are used for the precision determination of composition and thickness. This can be done also for each individual layer of multiple-layer films. 

An electron gun produces and accelerates the electron beam, which is reduced in diameter (demagnified) by one or more electromagnetic electron lenses. Electromagnetic scanning coils move this small electron probe (i.e., the beam) across the specimen in a raster. Electron detectors beyond the specimen collect a signal that is used to modulate the intensity on a cathode-ray tube that is scanned in synchronism with the beam on the specimen. A schematic of the essential components in a dedicated STEM system is shown in Figure 2. 

Here Pyj is the structure factor for the (hkl) diffiaction peak and is related to the atomic arrangements in the material. Specifically, Fjjj is the Fourier transform of the positions of the atoms in one unit cell. Each atom is weighted by its form factor, which is equal to its atomic number Z for small 26, but which decreases as 2d increases. Thus, XRD is more sensitive to high-Z materials, and for low-Z materials, neutron or electron diffraction may be more suitable. The faaor e (called the Debye-Waller factor) accounts for the reduction in intensity due to the disorder in the crystal, and the diffracting volume V depends on p and on the film thickness. For epitaxial thin films and films with preferred orientations, the integrated intensity depends on the orientation of the specimen. 

Interdiffusion of bilayered thin films also can be measured with XRD. The diffraction pattern initially consists of two peaks from the pure layers and after annealing, the diffracted intensity between these peaks grows because of interdiffusion of the layers. An analysis of this intensity yields the concentration profile, which enables a calculation of diffusion coefficients, and diffusion coefficients cm /s are readily measured. With the use of multilayered specimens, extremely small diffusion coefficients (-10 cm /s) can be measured with XRD. Alternative methods of measuring concentration profiles and diffusion coefficients include depth profiling (which suffers from artifacts), RBS (which can not resolve adjacent elements in the periodic table), and radiotracer methods (which are difficult). For XRD (except for multilayered specimens), there must be a unique relationship between composition and the d-spacings in the initial films and any solid solutions or compounds that form this permits calculation of the compo-... 

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