Calibration of a heating/cooling chamber for X-ray diffraction measurements of mechanical stress and crystallographic texture

2006 ◽  
Vol 39 (2) ◽  
pp. 194-201 ◽  
Author(s):  
M. Wohlschlögel ◽  
U. Welzel ◽  
G. Maier ◽  
E. J. Mittemeijer

Methods have been developed for the calibration of specimen temperature and of specimen displacement caused by the thermal expansion of the specimen holder in a heating/cooling chamber equipped with a strip or plate heater mounted on an X-ray diffractometer. For the temperature calibration two methods were proposed. One method relies on X-ray diffraction measurements of thermal lattice strains, whereas the other method is based on resistance thermometry. The method proposed for the determination of the temperature-dependent specimen displacement is based on the measurement of diffraction-line positions of the specimen employing two diffraction geometries, one being sensitive to the specimen displacement and the other being insensitive to the specimen displacement. The thermal displacement of the specimen due to thermal expansion of the specimen holder is significant and was determined as about 38 µm per 100 K.

2006 ◽  
Vol 258-260 ◽  
pp. 316-321 ◽  
Author(s):  
Evgeny N. Selivanov ◽  
R.I. Gulyaeva ◽  
V.M. Chumarev ◽  
N.I. Selmenskikh

The iron and zinc calcium oxysulfides Ca3Fe4S3O6, CaFeSO and CaZnSO are synthesized by reacting mixtures of CaO and FeS or of CaO and ZnS in an inert atmosphere. Their elemental compositions and lattice parameters are determined by X-ray microanalysis and X-ray diffraction. From the temperature-dependent lattice parameters of oxysulfides (measured up to 1170K) their thermal expansion coefficients are evaluated. Oxidation Ca3Fe4S3O6 and CaZnSO are studied by thermogravimetric analysis when air heated. Oxidation speed temperature coefficients showing that process limiting stage is diffusion are determined.


1997 ◽  
Vol 505 ◽  
Author(s):  
G. Cornella ◽  
S. Lee ◽  
O. Kraft ◽  
W. D. Nix ◽  
J. C. Bravman

ABSTRACTX-ray strain analysis via Generalized Focusing Diffractometry (GFD) [1], and the concurrent need for accurate values of the unstrained lattice parameter, are discussed. A new method for determining the unstrained lattice parameter without knowledge of the elastic constants of the sample material is described. Stress measurements at varying temperatures, and extraction of the coefficient of thermal expansion from these measurements, are demonstrated for aluminum and gold films.


2011 ◽  
Vol 26 (S1) ◽  
pp. S44-S46 ◽  
Author(s):  
Kenny Ståhl ◽  
Bastian Brink ◽  
Jonas Andersen

The structure of [Al2(pydc)2(μ2-OH)2(H2O)2]n(pydc = 2,5-pyridinedicarboxylate) was successfully determined from powder X-ray diffraction data. The compound crystallizes in the triclinic system (space group P -1) with a = 6.7813(1) Å, b = 7.4944(1) Å, c = 8.5013(1) Å, α = 95.256(1)°, β = 102.478(1)°, γ = 108.979(1)°. The structure consists of aluminum ions coordinating N and O in distorted octahedra, sharing an edge through two hydroxide ions. These dinuclear complexes are connected by pydc ions, which at one end coordinate by nitrogen and oxygen and only by oxygen at the other end. The pydc orientation is reversed in the neighboring pydc, forming double stranded chains interconnected by the aluminum dinuclear complexes in a ladder-like arrangement along [001].


2016 ◽  
Vol 49 (5) ◽  
pp. 1632-1644 ◽  
Author(s):  
Andreas Leineweber

Cementite (Fe3C) powder consisting of polycrystalline particles was investigated by synchrotron X-ray diffraction and neutron diffraction at temperatures between 10 and 973 K. The data reveal a pronouncedly anisotropic thermal expansion of the orthorhombic unit cell as well as microstrain broadening varying considerably with temperature. Using a theory for predicting thermal-microstress-induced microstrain already applied in previous work to ambient-temperature sealed-tube X-ray powder diffraction data from the same material [Leineweber (2012). J. Appl. Cryst. 45, 944–949], the temperature-dependent extent of the measured microstrain broadening could be quantitatively related to the measured temperature-dependent anisotropy of the thermal expansion. Thereby, the fact that the extent of the measured microstrain broadening is somewhat smaller than the predicted amount can be explained by the presence of the free surfaces of the powder particles reducing the level of microstress-induced microstrain.


2018 ◽  
Vol 212 ◽  
pp. 161-166 ◽  
Author(s):  
Adam C. Lindsey ◽  
Matthew Loyd ◽  
Maulik K. Patel ◽  
Ryan Rawl ◽  
Haidong Zhou ◽  
...  

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