Partial decomposition of TiH2 studied in situ by energy-dispersive diffraction and ex situ by diffraction microtomography of hard X-ray synchrotron radiation

2012 ◽  
Vol 66 (10) ◽  
pp. 757-760 ◽  
Author(s):  
C. Jiménez ◽  
F. Garcia-Moreno ◽  
A. Rack ◽  
R. Tucoulou ◽  
M. Klaus ◽  
...  
Keyword(s):  
Synchrotron Radiation ◽  
Energy Dispersive ◽  
Ex Situ ◽  
X Ray ◽  
Partial Decomposition ◽  
Energy Dispersive Diffraction

Instrumentation for Synchrotron X-Ray Powder Diffractometry

1985 ◽  
Vol 29 ◽  
pp. 243-250 ◽  
Author(s):  
W. Parrish ◽  
M. Hart ◽  
C. G. Erickson ◽  
N. Masciocchi ◽  
T. C. Huang
Keyword(s):  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
Storage Ring ◽  
Scintillation Counter ◽  
Diffraction Method ◽  
Energy Dispersive ◽  
Parallel Beam ◽  
X Ray ◽  
Radiation Laboratory ◽  
Energy Dispersive Diffraction

AbstractThe instrumentation developed for poly crystalline diffractometry using the storage ring at the Stanford Synchrotron Radiation Laboratory is described. A pair of automated vertical scan diffractometers was used for a Si (111) channel monochromator and the powder specimens. The parallel beam powder diffraction was defined by horizontal parallel slits which had several times higher intensity than a receiving slit at the same resolution. The patterns were obtained with 2:1 scanning with’ a selected monochromatic beam, and an energy dispersive diffraction method in which the monochromator is step-scanned, and the specimen and scintillation counter are fixed. Both methods use the same instrumentation.

A Combined Voltammetric and Synchrotron Radiation-Grazing Incidence X-ray Diffraction Study of the Electrocrystallization of Zinc Tetracyanoquinodimethane

2012 ◽  
Vol 65 (3) ◽  
pp. 236 ◽  
Author(s):  
Jean-Pierre Veder ◽  
Ayman Nafady ◽  
Graeme Clarke ◽  
Roland De Marco ◽  
Alan M. Bond
Keyword(s):  
Synchrotron Radiation ◽  
Grazing Incidence ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
Pt Electrode ◽  
Cyclic Voltammetric ◽  
X Ray ◽  
Ir And Raman ◽  
Voltammetric Peak

The in situ electrocrystallization of zinc tetracyanoquinodimethane (TCNQ) has been explored using synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) at potentials in the region of the cyclic voltammetric peak where reduction of TCNQ to TCNQ– occurs at a Pt electrode in acetonitrile (0.1 M [NBu4][PF6]) solution containing Zn(NO3)2·6H2O. The in situ SR-GIXRD data along with ex situ IR and Raman spectroscopy results all confirmed the formation of the kinetically favoured phase of Zn[TCNQ]2(H2O)2 as the product.

scholarly journals Energy-dispersive diffraction studies of inert anodes

2009 ◽  
Vol 42 (3) ◽  
pp. 502-512 ◽  
Author(s):  
Nicola V. Y. Scarlett ◽  
Ian C. Madsen ◽  
John S. O. Evans ◽  
Alan A. Coelho ◽  
Katherine McGregor ◽  
...  
Keyword(s):  
Energy Dispersive ◽  
Quantitative Phase Analysis ◽  
Electrochemical Cells ◽  
Electrolysis Time ◽  
X Ray Diffraction ◽  
X Ray ◽  
Inert Anodes ◽  
Lower Limits ◽  
Energy Dispersive Diffraction

A tomographic study of electrochemical cells to observe scales formed on inert anodes has been conducted using energy-dispersive synchrotron X-ray diffraction. This study is preparatory to an investigation that will observe this formationin situduring the cells' operation. The purpose of the current work was to determine whether this technique would be appropriate for such a study in terms of its sensitivity and whether the results could be quantified satisfactorily. A method has been developed for the quantitative phase analysis of energy-dispersive data using crystal-structure-based Rietveld refinement. This has been tested with standard materials and found to be comparable in accuracy to results obtained from traditional angular-dispersive diffraction. The lower limits of detection of the method have not been established quantitatively but qualitative differences can be seen between cells that have been cycled at different times. These differences indicate a linear relationship between scale formation and electrolysis time.

Metal Foaming Studied In Situ by Energy Dispersive X-Ray Diffraction of Synchrotron Radiation, X-Ray Radioscopy, and Optical Expandometry

2012 ◽  
Vol 15 (3) ◽  
pp. 141-148 ◽  
Author(s):  
Catalina Jiménez ◽  
Francisco Garcia-Moreno ◽  
Beate Pfretzschner ◽  
Paul Hans Kamm ◽  
Tillmann Robert Neu ◽  
...  
Keyword(s):  
Synchrotron Radiation ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
X Ray

Atomic Layer Deposition of LiF and Lithium Ion Conducting (AlF3)(LiF)x Alloys Using Trimethylaluminum, Lithium Hexamethyldisilazide and Hydrogen Fluoride

2017 ◽  
Author(s):  
Younghee Lee ◽  
Daniela M. Piper ◽  
Andrew S. Cavanagh ◽  
Matthias J. Young ◽  
Se-Hee Lee ◽  
...  
Keyword(s):  
Lithium Ion ◽  
Atomic Layer ◽  
Mass Gain ◽  
Alloy Film ◽  
Ex Situ ◽  
X Ray ◽  
Layer Deposition ◽  
Ion Conducting ◽  
Good Agreement

<div>Atomic layer deposition (ALD) of LiF and lithium ion conducting (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloys was developed using trimethylaluminum, lithium hexamethyldisilazide (LiHMDS) and hydrogen fluoride derived from HF-pyridine solution. ALD of LiF was studied using in situ quartz crystal microbalance (QCM) and in situ quadrupole mass spectrometer (QMS) at reaction temperatures between 125°C and 250°C. A mass gain per cycle of 12 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH<sub>3</sub>)<sub>3</sub> as a reaction byproduct instead of HMDS at 150°C. LiF ALD showed self-limiting behavior. Ex situ measurements using X-ray reflectivity (XRR) and spectroscopic ellipsometry (SE) showed a growth rate of 0.5-0.6 Å/cycle, in good agreement with the in situ QCM measurements.</div><div>ALD of lithium ion conducting (AlF3)(LiF)x alloys was also demonstrated using in situ QCM and in situ QMS at reaction temperatures at 150°C A mass gain per sequence of 22 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C. Ex situ measurements using XRR and SE showed a linear growth rate of 0.9 Å/sequence, in good agreement with the in situ QCM measurements. Stoichiometry between AlF<sub>3</sub> and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF<sub>3</sub>)(LiF)x alloy consists of aluminum, lithium and fluorine. Carbon, oxygen, and nitrogen impurities were both below the detection limit of XPS. Grazing incidence X-ray diffraction (GIXRD) observed that LiF and (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film have crystalline structures. Inductively coupled plasma mass spectrometry (ICP-MS) and ionic chromatography revealed atomic ratio of Li:F=1:1.1 and Al:Li:F=1:2.7: 5.4 for (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film was measured as σ = 7.5 × 10<sup>-6</sup> S/cm.</div>

In Situ X-Ray Diffraction Investigations during Diffusion Anneals of Ni-Cu Thin Film Diffusion Couples

2010 ◽  
Vol 89-91 ◽  
pp. 503-508 ◽  
Author(s):  
J. Sheng ◽  
U. Welzel ◽  
Eric J. Mittemeijer
Keyword(s):  
Thermal Stresses ◽  
Stress Generation ◽  
Ex Situ ◽  
Diffusion Annealing ◽  
X Ray Diffraction ◽  
Individual Layer ◽  
X Ray ◽  
Bilayer System ◽  
Stress Changes

The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.

In situ X-ray Scattering Study of the Formation of Au Nano Crystals During Thermal Annealing

2007 ◽  
Vol 1027 ◽  
Author(s):  
Do Young Noh ◽  
Ki-Hyun Ryu ◽  
Hyon Chol Kang
Keyword(s):  
Thermal Annealing ◽  
Bragg Reflection ◽  
Ex Situ ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Au Thin Films ◽  
Ray Scattering

AbstractThe transformation of Au thin films grown on sapphire (0001) substrates into nano crystals during thermal annealing was investigated by in situ synchrotron x-ray scattering and ex situ atomic force microscopy (AFM). By monitoring the Au(111) Bragg reflection and the low Q reflectivity and comparing them with ex situ AFM images, we found that polygonal-shape holes were nucleated and grow initially. As the holes grow larger and contact each other, their boundary turns into Au nano crystals. The Au nano crystals have a well-defined (111) flat top surface and facets in the in-plane direction.

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