X-ray diffraction films

The original and still useful method of X-ray detection is the exposure of photographic film. In the early days of X-ray diffraction, films were also used for the quantitative recording of X-ray intensities. Densitometer measurements of optical density, D, were made of the film. The optical density is defined by... 

This lamp also illuminates, through a focusing optical system, a small region of the x-ray diffraction film. The transmitted... 

The crystals of space group Pna2i have a relatively large unit cell, containing Z = 12 units RE Na(Si04) (Table 6). The structure of NaNd(Si04) was determined from three-dimensional X-ray diffraction film data and refined to an R value of 13% (55). Individual temperatures were not reported in (55). 

There is a fair amount of work reported with films at the mercury-air interface. Rice and co-workers [107] used grazing incidence x-ray diffraction to determine that a crystalline stearic acid monolayer induces order in the Hg substrate. Quinone derivatives spread at the mercury-n-hexane interface form crystalline structures governed primarily by hydrogen bonding interactions [108]. 

For bulk structural detemiination (see chapter B 1.9). the main teclmique used has been x-ray diffraction (XRD). Several other teclmiques are also available for more specialized applications, including electron diffraction (ED) for thin film structures and gas-phase molecules neutron diffraction (ND) and nuclear magnetic resonance (NMR) for magnetic studies (see chapter B1.12 and chapter B1.13) x-ray absorption fine structure (XAFS) for local structures in small or unstable samples and other spectroscopies to examine local structures in molecules. Electron microscopy also plays an important role, primarily tlirough unaging (see chapter B1.17). 

Tredgold R H, Allen R A and Hodge P 1987 X-ray-diffraction and optical studies of Langmuir-Blodgett films formed from azobenzene derivatives Thin Solid Films 155 343-52... 

The value for the heat of fusion of PPS, extrapolated to a hypothetical 100% crystalline state, is not agreed upon in the literature. Reported values range from approximately 80 J/g (19 cal/g) (36,96,101) to 146 J/g (35 cal/g) (102), with one intermediate value of 105 J/g (25 cal/g) (20). The lower value, 80 J/g, was originally measured by thermal analysis and then correlated with a measure of crystallinity deterrnined by x-ray diffraction (36). The value of 146 J/g was deterrnined independendy on uniaxiaHy oriented PPS film samples by thermal analysis, density measurement via density-gradient column, and the use of a calculated density for 100% crystalline PPS to arrive at a heat of fusion for 100% crystalline PPS (102). The value of 105 J/g was obtained by measuring the heats of fusion of weU-characterized linear oligomers of PPS and extrapolation to infinite molecular weight. 

X-ray diffraction consists of the measurement of the coherent scattering of x-rays (phenomenon 4 above). X-ray diffraction is used to determine the identity of crystalline phases in a multiphase powder sample and the atomic and molecular stmctures of single crystals. It can also be used to determine stmctural details of polymers, fibers, thin films, and amorphous soflds and to study stress, texture, and particle size. 

This chapter contains articles on six techniques that provide structural information on surfaces, interfeces, and thin films. They use X rays (X-ray diffraction, XRD, and Extended X-ray Absorption Fine-Structure, EXAFS), electrons (Low-Energy Electron Diffraction, LEED, and Reflection High-Energy Electron Diffraction, RHEED), or X rays in and electrons out (Surfece Extended X-ray Absorption Fine Structure, SEXAFS, and X-ray Photoelectron Diffraction, XPD). In their usual form, XRD and EXAFS are bulk methods, since X rays probe many microns deep, whereas the other techniques are surfece sensitive. There are, however, ways to make XRD and EXAFS much more surfece sensitive. For EXAFS this converts the technique into SEXAFS, which can have submonolayer sensitivity. 

X-ray Diffraction (XRD) is a powerful technique used to uniquely identify the crystalline phases present in materials and to measure the structural properties (strain state, grain size, epitaxy, phase composition, preferred orientation, and defect structure) of these phases. XRD is also used to determine the thickness of thin films and multilayers, and atomic arrangements in amorphous materials (including polymers) and at inter ces. 

For ultrathin epitaxial films (less than "100 A), Grazingincidence X-ray Diffraction (GrXD) is the preferred method and has been used to characterize monolayer films. Here the incidence angle is small ("0.5°) and the X rays penetrate only "100-200 A into the specimen (see below). The exit angle of the diffracted X rays is also small and structural information is obtained about (hkl) planes perpendicular to the specimen sur e. Thus, GIXD complements those methods where structural information is obtained about planes parallel to the surface (e.g., Bra -Brentano and DCD). 

A. SegmuUer and M. Murakami. Characterization of Thin Films by X-Ray Diffraction. In Thin Films from Free Atoms and Particles. (K.J. Kla-bunde, ed.) Academic Press, Orlando, 1985, p.325 A recent brief review article with many references. 

A. Segmuller, I, C. Noyan, V. S. Speriosu. X-Ray Diffraction Studies of Thin Films and Multilayer Structures. Prog. Cryst. Growth and Charact. 18,21, 1989. 

A. Segmuller and M. Murakami. X-Ray Diffraction Analysis of Strains and Stresses in Thin Films. In Analytical Techniques for Thin Films. (K.N. Tu and R. Rosenberg, eds.) Academic, San Diego, 1988, p.l43. 

Some of the techniques included apply more broadly than just to surfaces, interfaces, or thin films for example X-Ray Diffraction and Infrared Spectroscopy, which have been used for half a century in bulk solid and liquid analysis, respectively. They are included here because they have by now been developed to also apply to surfaces. A few techniques that are applied almost entirely to bulk materials (e.g.. Neutron Diffraction) are included because they give complementary information to other methods or because they are referred to significantly in the 10 materials volumes in the Series. Some techniques were left out because they were considered to be too restricted to specific applications or materials. 

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