In-situ dehydration studies of fully K-, Rb-, and Cs-exchanged natrolites

In-situ synchrotron X-ray powder diffraction studies of K-, Rb-, and Cs-exchanged natrolites between room temperature and 425 °C revealed that the dehydrated phases with collapsed frameworks start to form at 175, 150, and 100 °C, respectively. The degree of the framework collapse indicated by the unit-cell volume contraction depends on the size of the non-framework cation: K-exchanged natrolite undergoes an 18.8% unit-cell volume contraction when dehydrated at 175 °C, whereas Rb- and Cs-exchanged natrolites show unit-cell volume contractions of 18.5 and 15.2% at 150 and 100 °C, respectively. In the hydrated phases, the dehydration-induced unit-cell volume reduction diminishes as the cation size increases and reveals increasingly a negative slope as smaller cations are substituted into the pores of the natrolite structure. The thermal expansion of the unit-cell volumes of the dehydrated K-, Rb-, and Cs-phases have positive thermal expansion coefficients of 8.80 × 10⁻⁵ K⁻¹, 1.03 × 10⁻⁴ K⁻¹, and 5.06 × 10⁻⁵ K⁻¹, respectively. Rietveld structure refinements of the dehydrated phases at 400 °C reveal that the framework collapses are due to an increase of the chain rotation angles, ψ, which narrow the channels to a more elliptical shape. Compared to their respective hydrated structures at ambient conditions, the dehydrated K-exchanged natrolite at 400 °C shows a 2.2-fold increase in ψ, whereas the dehydrated Rb- and Cs-natrolites at 400 °C reveal increases of ψ by ca. 3.7 and 7.3 times, respectively. The elliptical channel openings of the dehydrated K-, Rb-, to Cs-phases become larger as the cation size increases. The disordered non-framework cations in the hydrated K-, Rb-, and Cs-natrolite order during dehydration and the subsequent framework collapse. The dehydrated phases of Rb- and Cs-natrolite can be stabilized at ambient conditions.

In-situ white beam microdiffraction study of the deformation behavior in polycrystalline magnesium alloy during uniaxial loading

Scanning white beam X-ray microdiffraction has been used to study the heterogeneous grain deformation in a polycrystalline Mg alloy (MgAZ31). The high spatial resolution achieved on beamline 7.3.3 at the Advanced Light Source provides a unique method to measure the elastic strain and orientation of single grains as a function of applied load. To carry out in-situ measurements a light weight (~0.5kg) tensile stage, capable of providing uniaxial loads of up to 600kg, was designed to collect diffraction data on the loading and unloading cycle. In-situ observation of the deformation process provides insight about the crystallographic deformation mode via twinning and dislocation slip.

In-situ studies of X-ray diffraction line profiles from strained copper foils

The development of an in-situ tensometer is described along with preliminary results of x-ray line profiles from copper foils under tensile stress. The tensometer was designed and constructed on the high resolution diffraction instrument, Station 2.3 at the synchrotron radiation source (SRS) Daresbury Laboratory, and is capable of collecting data in either symmetric or asymmetric geometry including transmission and reflection modes. Experiments were carried out using 18 J..Lm thick copper foil up to strain levels of 5 % using both symmetric reflection and symmetric transmission diffraction. All profiles displayed diffraction broadening and asymmetry which increased with strain. In addition, the asymmetry observed in symmetric transmission was associated with extended tails on the low angle side of the profiles, but in symmetric reflection data the opposite asymmetry was observed. In the analysis, the measured profiles were fitted using the software TOPAS, a fundamental parameters approach to profile fitting. The instrumental profile function was characterised and modelled using annealed LaB6 powder. The diffraction broadening was then determined by refining the convolution of a Voigt function, an asymmetric exponential function and a fixed instrument function to reproduce the observed broadened profiles. The integral breadth and asymmetry results display a strong order dependence and increase almost linearly with strain. The results were interpreted by assuming crystallite size broadening in combination with dislocation broadening arising from fcc a/2( 110) {Ill } dislocations.