From ultra-high vacuum to the electrochemical interface: X-ray scattering studies of model electrocatalysts

2009 ◽  
Vol 140 ◽  
pp. 41-58 ◽  
Author(s):  
Christopher A. Lucas ◽  
Michael Cormack ◽  
Mark E. Gallagher ◽  
Alexander Brownrigg ◽  
Paul Thompson ◽  
...  
1993 ◽  
Vol 37 ◽  
pp. 413-418
Author(s):  
Joanne Levine Parrill ◽  
Jerome B. Cohen ◽  
Yip-Wah Chung

AbstractAn ultra-high vacuum chamber designed for in situ grazing incidence small angle x-ray scattering (GISAXS) surface analysis is described. Unique features of this equipment are the precision rotary feedthrough for angular alignment of the sample, the sample heating design, the Be window arrangement, and the compatibility of this chamber with both a rotating anode and a synchrotron beamline. This chamber was used as part of a GISAXS camera utilizing a 18 kW Rigaku rotating anode, pin-hole collimation, and a position sensitive detector. The resolution of this camera was 0.007 A-1 with a 1.4 mm wide beamstop and CuKα


2013 ◽  
Vol 20 (3) ◽  
pp. 474-481 ◽  
Author(s):  
Pilar Ferrer ◽  
Juan Rubio-Zuazo ◽  
Catherine Heyman ◽  
Fatima Esteban-Betegón ◽  
Germán R. Castro

The multipurpose portable ultra-high-vacuum-compatible chamber described in detail in this article has been designed to carry out grazing-incidence X-ray scattering techniques on the BM25-SpLine CRG beamline at the ESRF. The chamber has a cylindrical form, built on a 360° beryllium double-ended conflate flange (CF) nipple. The main advantage of this chamber design is the wide sample temperature range, which may be varied between 60 and 1000 K. Other advantages of using a cylinder are that the wall thickness is reduced to a minimum value, keeping maximal solid angle accessibility and keeping wall absorption of the incoming X-ray beam constant. The heat exchanger is a customized compact liquid-nitrogen (LN2) continuous-flow cryostat. LN2 is transferred from a storage Dewar through a vacuum-isolated transfer line to the heat exchanger. The sample is mounted on a molybdenum support on the heat exchanger, which is equipped with a BORALECTRIC heater element. The chamber versatility extends to the operating pressure, ranging from ultra-high vacuum (<10−10 mbar) to high pressure (up to 3 × 103 mbar). In addition, it is equipped with several CF ports to allocate auxiliary components such as capillary gas-inlet, viewports, leak valves, ion gun, turbo pump,etc., responding to a large variety of experiment requirements. A movable slits set-up has been foreseen to reduce the background and diffuse scattering produced at the beryllium wall. Diffraction data can be recorded either with a point detector or with a bi-dimensional CCD detector, or both detectors simultaneously. The system has been designed to carry out a multitude of experiments in a large variety of environments. The system feasibility is demonstrated by showing temperature-dependence grazing-incidence X-ray diffraction and conductivity measurements on a 20 nm-thick La0.7Ca0.3MnO3thin film grown on a SrTiO3(001) substrate.


Author(s):  
A. R. Modak ◽  
David J. Smith ◽  
Z. G. Li ◽  
P. Boher ◽  
Ph. Houdy

Multilayers fabricated with alternating materials having significant differences in X-ray scattering powers are being investigated for applications in soft X-ray optics. Multilayers consisting of combinations of W, Rh, Fe, Si3N4, SiO2 and Si, C, B4C have been studied in the past. Mg2Si based multilayer structures are theoretically efficient reflectors of wavelengths above the Mg-Kα line (9.89 Å) and the Mg-Lα line (251.5 Å) because of their low absorption in the respective wavelength regimes due to the presence of magnesium. In the present study, Mg2Si based multilayers fabricated on silicon substrates by ultra high vacuum rf sputtering have been characterized by HREM. W, Si, and Mg2Si targets in conjunction with the introduction of nitrogen were employed to deposit alternate Mg2Si and W or Si3N4 layers. We report here our preliminary observations of a characteristic short period W/Mg2Si layered structure used above the Mg-Kα line and two long period multilayers based on W/Mg2Si and Si3N4/Mg2Si used above the Mg-Lα line.


2012 ◽  
Vol 83 (8) ◽  
pp. 083904 ◽  
Author(s):  
F. Bertram ◽  
C. Deiter ◽  
K. Pflaum ◽  
O. H. Seeck

Author(s):  
Eva-Maria Mandelkow ◽  
Eckhard Mandelkow ◽  
Joan Bordas

When a solution of microtubule protein is changed from non-polymerising to polymerising conditions (e.g. by temperature jump or mixing with GTP) there is a series of structural transitions preceding microtubule growth. These have been detected by time-resolved X-ray scattering using synchrotron radiation, and they may be classified into pre-nucleation and nucleation events. X-ray patterns are good indicators for the average behavior of the particles in solution, but they are difficult to interpret unless additional information on their structure is available. We therefore studied the assembly process by electron microscopy under conditions approaching those of the X-ray experiment. There are two difficulties in the EM approach: One is that the particles important for assembly are usually small and not very regular and therefore tend to be overlooked. Secondly EM specimens require low concentrations which favor disassembly of the particles one wants to observe since there is a dynamic equilibrium between polymers and subunits.


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