Carbon diffraction

Prompted by the success, TOFD measurements were conducted on a fatigue crack in a stainless steel compact tension specimen. Test and system parameters were optimised following the same procedure used for carbon steel specimens. A clear diffracted signal was observed with relatively good SNR and its depth as measured from the time-of-flight measurements matched exactly with the actual depth. 

The tnhahdes of phosphoms usually are obtained by direct halogenation under controlled conditions, eg, in carbon disulfide solution in the case of the triiodide. Phosphoms trifluoride [7647-19-0] is best made by transhalogenation of PCl using AsF or Cap2. AH of the phosphoms tnhahdes are both Lewis bases and acids. The phosphoms tnhahdes rapidly hydroly2e in water and are volatile. Examination by electron diffraction has confirmed pyramidal stmctures for the gaseous tnhahde molecules (36). Physical properties and heat of formation of some phosphoms hahdes are hsted in Table 7. 

These hydrated salts contain bidentate carbonate ligands and no water molecules are bound directly to the central metal atom. The only single-crystal x-ray diffraction studies available are those for salts of (4) (52—54) and the mineral tuliokite [128706 2-3], Na2BaTh(C03)2 -6H20], which contains the unusual Th(C02) 2 anion (5) (55). 

The stmcture of activated carbon is best described as a twisted network of defective carbon layer planes, cross-linked by aHphatic bridging groups (6). X-ray diffraction patterns of activated carbon reveal that it is nongraphitic, remaining amorphous because the randomly cross-linked network inhibits reordering of the stmcture even when heated to 3000°C (7). This property of activated carbon contributes to its most unique feature, namely, the highly developed and accessible internal pore stmcture. The surface area, dimensions, and distribution of the pores depend on the precursor and on the conditions of carbonization and activation. Pore sizes are classified (8) by the International Union of Pure and AppHed Chemistry (lUPAC) as micropores (pore width <2 nm), mesopores (pore width 2—50 nm), and macropores (pore width >50 nm) (see Adsorption). 

Crystal Structure. Diamonds prepared by the direct conversion of well-crystallized graphite, at pressures of about 13 GPa (130 kbar), show certain unusual reflections in the x-ray diffraction patterns (25). They could be explained by assuming a hexagonal diamond stmcture (related to wurtzite) with a = 0.252 and c = 0.412 nm, space group P63 /mmc — Dgj with four atoms per unit cell. The calculated density would be 3.51 g/cm, the same as for ordinary cubic diamond, and the distances between nearest neighbor carbon atoms would be the same in both hexagonal and cubic diamond, 0.154 nm. 

The composition varies with the heat treatment and the end point according to x-ray diffraction studies it is a form of carbon that reconverts to weU-ordered graphite on heating to 1800°C. Before the use of x-rays, chemists used the Brodie reaction to differentiate between graphitic carbons and turbostratic carbons. Turbostratic carbons yield a brown solution of humic acids, whereas further oxidation of graphite oxide produces mellitic acid (benzenehexacarboxyhc acid) [517-60-2] ... 

The simplest analytical procedure is to oxidize a sample in air below the fusion point of the ash. The loss on ignition is reported as graphitic carbon. Refinements are deterrninations of the presence of amorphous carbon by gravity separation with ethylene bromide, or preferably by x-ray diffraction, and carbonates by loss of weight on treating with nitric acid. Corrections for amorphous carbon and carbonates are appHed to the ignition data, but loss of volatile materials and oxidation may introduce errors. 

The hydrated alumina minerals usually occur in ooUtic stmctures (small spherical to eUipsoidal bodies the size of BB shot, about 2 mm in diameter) and also in larger and smaller stmctures. They impart harshness and resist fusion or fuse with difficulty in sodium carbonate, and may be suspected if the raw clay analyzes at more than 40% AI2O2. Optical properties are radically different from those of common clay minerals, and x-ray diffraction patterns and differential thermal analysis curves are distinctive. 

Physical Methods of Examination. Physical methods used to examine coals can be divided into two classes which, in the one case, yield information of a stmctural nature such as the size of the aromatic nuclei, ie, methods such as x-ray diffraction, molar refraction, and calorific value as a function of composition and in the other case indicate the fraction of carbon present in aromatic form, ie, methods such as ir and nuclear magnetic resonance spectroscopies, and density as a function of composition. Some methods used and types of information obtained from them are (41) ... 

Structural parameters and interatomic distances derived from electron diffraction (7) (77JST(42)l2i) and X-ray diffraction (8) studies (76AX(B)3178) provide unequivocal evidence that pyrazine is planar with >2a symmetry. There is an increased localization of electron density in the carbon-nitrogen bonds, with carbon-carbon bonds being similar in length to those in benzene. ... 

X-ray diffraction peaks were rather broad with coherence lengths as low as 20 nm and this was attributed to rapid quenching. It was proposed that the carbon atoms are arranged in polyyne chains (n = 4) along the c-axis. The density of Carbolite (1.46 g-cm ) is lower than values for other carbynes and for diamond and graphite - hence the name - and this was attributed to a rapid quenching process. 

Despite many publications on carbynes, their existence has not been universally accepted and the literature has been characterised by conflicting claims and counter claims [e.g., 27-29]. This is particularly tme of meteoritic carbynes. An interesting account of die nature of elemental carbon in interstellar dust (including diamond, graphite and carbynes) was given by Pillinger [30]. Reitmeijer [31] has re-interpreted carbyne diffraction data and has concluded that carbynes could be stratified or mixed layer carbons with variable heteroelement content (H,0,N) rather than a pure carbon allotrope. 

In addition to questions over interpretation of diffraction data, diere are reservations about the stability of carbynes. Lagow et al [32] note that the condensation of the compound Li-C=C-Br to form carbon chains is potentially explosive. There is also the possibility of cross-linking between carbyne chains and the nature of the termination of the carbyne chains is unclear. Eastmond et al [33] showed that polyyne compounds of the type ... 

It is beyond the scope of this chapter to review structure and bonding in each class of engineering carbons listed in Table 5. Instead, a generic description of microstructure and bonding in these materials will be attempted. The evolution in understanding of the structure of engineering carbons and graphites has followed the initial application of X-ray diffraction and subsequent application... 

In the 1930s Hoffman and Wilm [101] found only (hkO) graphite reflections in an x-ray diffraction study of a carbon black. The absence of graphitie (hkl) reflections led them to propose a structure consisting of graphitic carbon layer... 

Pings [106], and a neutron diffraction study by Mildner and Carpenter [107], both concluded that there is no clear evidence for sp carbon and that the radial distribution functions can be satisfactorily indexed to a hexagonal arrays of carbon atoms. A similar conclusion was reached in a recent neutron diffraction study of activated carbons by Gardner et al [108]. 

Suzuki, T. and Kaneko, K., Structural change of activated carbon fibers with desorption by in situ x-ray diffraction. Carbon, 1988, 26(5), 744 745. 

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