In situ X-ray diffraction

Koop T, Schindler W, Kazimirov A, Scherb G, Zegenhagen J, Schulz T, Feidenhans l R and Kirschner J 1998 Electrochemical cell tor in situ x-ray diffraction under ultrapure conditions Rev. Sc/, instrum. 69 1840... 

Li J and Abruna FI D 1997 Coadsorption of sulphate/bisulphate anions with Fig cations during Fig underpotential deposition on Au (111) An In situ x-ray diffraction study J. Phys. Chem. B 101 244-52... 

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. 

Experimentally, different structure- and surface-sensitive techniques such as in situ scanning tunnelling microscopy (STM), in situ X-ray diffraction (XRD), transition electron microscopy (TEM), and in situ infrared (IR) spectroscopy have been... 

Lucas CA, Markovic NM. 2006. In-situ X-ray diffraction studies of the electrode/solution interface. In AUdre RC, Kolb DM, Lipkowski J, Ross PN, editors. Advances in Electrochemical Science and Engineering. Volume 9. New York Wiley-VCH, pp. 1-45. 

The effects of tin/palladium ratio, temperatnre, pressnre, and recycling were studied and correlated with catalyst characterization. The catalysts were characterized by chemisorption titrations, in situ X-Ray Diffraction (XRD), and Electron Spectroscopy for Chemical Analysis (ESCA). Chemisorption studies with hydrogen sulfide show lack of adsorption at higher Sn/Pd ratios. Carbon monoxide chemisorption indicates an increase in adsorption with increasing palladium concentration. One form of palladium is transformed to a new phase at 140°C by measurement of in situ variable temperature XRD. ESCA studies of the catalysts show that the presence of tin concentration increases the surface palladium concentration. ESCA data also indicates that recycled catalysts show no palladium sulfide formation at the surface but palladium cyanide is present. 

A number of surface diffraction techniques can be employed in the structural study of electrochemical interfaces, depending on the details of the system under study. For bulk materials or thick films (such that the X-ray beam only samples that layer) conventional diffraction experiments can be performed and, in fact, a number of in situ X-ray diffraction studies of this type have been reported.126 129 In the case of thin films or monolayers, two different techniques can be employed and these are the reflection-diffraction technique introduced by Marra and Eisenberger,3 ), 32 and the technique based on surface truncation rods.131 In the first case, the incident X-ray beam impinges on the sample at an angle below... 

In-situ x-ray diffraction (XRD) was performed on a coin type cell with a 4x6 mm Kapton window coated with conductive thin copper layer. The graphite electrode was pressed against the Kapton window so as to be reached by the x-ray beam. After several lithiation/delithiation cycles under a C/10 rate between 1.5 and 0V, the cell was fully delithiated up to 1.5V. The cycle capacity achieved with the graphite electrode is about 360mAh/g. The cell was then re-lithiated under a slower rate of C/20. XRD patterns were taken for about five minutes every hour while the cell is under continuous discharge. As result the lithium composition x in LixC6 was incremented by 0.05 between two successive XRD scans. 

Fransson L. M. L, Vaughey J. T., Benedek R., Edstrom K., Thomas J. O., Thackeray M. M., Phase transitions in lithiated Cu2Sb anodes for lithium batteries an in situ X-ray diffraction study, Electrochem. Commun., (2001) 3 (7), 317-323. 

Aspects of X-ray diffraction on single spider fibres. Int.J. Biol. Macromol. 24,179-186. Riekel, C., Mueller, M., and Vollrath, F. (1999b). In situ X-ray diffraction during forced silking of spider silk. Macromolecules 32, 4464-4466. 

M. M. Gunter, T. Ressler, R. E. lentoft, and B. Bems, Redox behavior of copper oxide catalysts in the steam reforming of methanol studied by in situ X-ray diffraction and absorption spectroscopy, J. Catal. 203, 133-149 (2001). 

D. Sun, F. Gingl, Y. Nakamura, H. Enoki, M. Bououdina, E. AMba, In situ X-ray diffraction study of hydrogen-induced phase decomposition in LaMg and La Mg, J. Alloys Compd. 333 (2002) 103-108. 

G. Sandrock, K. Gross, G.J. Thomas, Dynamic in situ X-ray diffraction of catalyzed alanates , J. Alloys Compd. 330-332 (2002) 691-695. 

The direct evidence that Besenhard et al. presented for the formation of a ternary GIC is the dilatometric measurement of the graphite electrode, which indicates a crystal expansion of 150% at the cointercalation potential. However, this expansion due to solvent cointercalation was never confirmed on the microscopic level. All of the in situ X-ray diffraction (XRD) measurements conducted by different research-... 

For in situ x-ray diffraction measurements, the basic construction of an electrochemical cell is a cell-type enclosure of an airtight stainless steel body. A beryllium window, which has a good x-ray transmission profile, is fixed on an opening in the cell. The cathode material can be deposited directly on the beryllium window, itself acting as a positive-electrode contact. A glass fiber separator soaked in liquid electrolyte is then positioned in contact with the cathode followed by a metal anode (3). A number of variations and improvements have been introduced to protect the beryllium window, which is subject to corrosion when the high-voltage cathode is in direct contact with it. 

In Situ X-ray Diffraction Measurements of the Self-Preservation Effect of CH4 Hydrate. J. Phys. Chem. A, 105, 9756-9759. 

Meyer B, Ziemer B, Scholz F (1995) In Situ X-ray diffraction study of the electrochemical reduction of tetragonal lead oxide and orthorhombic Pb(OH)Cl mechanically immobilized on a graphite electrode. J Electroanal Chem 392 79-83. 

Non-stoichiometry, which originates from various kinds of lattice defect, can be derived from the phase rule. As an introduction, let us consider a trial experiment to understand non-stoichiometry (this experiment is, in principle, analogous to the one described in Section 1.4.8). Figure 1.1 shows a reaction vessel equipped with a vacuum pump, pressure gauge for oxygen gas, pressure controller for oxygen gas, thermometer, and chemical balance. The temperature of the vessel is controlled by an outer-furnace and the vessel has a special window for in-situ X-ray diffraction. A quantity of metal powder... 

A more recent study has examined the SH response from a Au(lll) electrode during UPD of a variety of metals, Ag, Cu, Pb, T1 and Sb [155]. In situ x-ray diffraction techniques have examined Ag, Cu and Pb on this substrate [159-161]. Silver is shown to form an epitaxial overlayer with Ag atoms sitting in 3-fold hollow sites forming a (1X1) commensurate overlayer. The lattice mismatch between lead and the substrate is shown to prevent formation of a commensurate overlayer but forms a hexagonal close-packed overlayer contracted by 0.7% from bulk lead. Although T1 and Sb on Au (111) have not been examined by x-ray diffraction, a close packed structure would necessitate an incommensurate overlayer due to the lattice mismatch. 

Courtney IA, Dahn JR. Electrochemical and in situ X-ray diffraction studies of the reaction of lithium with Tin oxide composites. J Electrochem Soc 1997 144 2045-2052. 

The in situ X-ray diffraction [89, 97] data further excluded the possibility that oxygen intercalates between the graphene layers and starts the reaction in a... 

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