In situ waxs-saxs synchrotron study of the kinetics of nucleation and growth in linde type-a zeolite (LTA)

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Abstract

Wide-angle and small-angle scattering investigations on the templated nucleation and growth processes of Linde Type-A zeolite from clear solution were performed in situ using synchrotron radiation and small volume reaction cells. The selected system contains TMAOH as the organic templating agent.

Full kinetic analysis of the isothermal data was performed and the resulting kinetic parameters indicate that the nucleation mechanism can not be described as an entirely homogeneous crystallization process from solution. The small angle scattering data show the development and evolution of two distinct particle populations during the crystallization process. They are interpreted according to a mechanism of formation of α-cage structural units attaching directly to the surface of the growing zeolite crystallites.

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      In the past, efforts to analyze the crystallization of zeolites in real-time have been undertaken on the lab scale with focus on mechanisms rather than particle size. Different analytical methods, such as electrochemical methods/conductivity [10,11], viscosity measurements [12], calorimetry [13], spectroscopic methods [14] (IR [15,16], Raman [17–19], NMR [20,21], X-Ray absorption (XANES, EXAFS) [22]), mass spectrometry [23], and X-ray powder diffraction (XRD) [24–26] as well as X-ray scattering (SAXS, WAXS) [22,27–29], have been employed. To the best of our knowledge, only two publications report on inline spectroscopic methods applicable in pilot or production scale (IR spectroscopy [30], Raman spectroscopy [31]), whereas all others are based on specially designed at-/off-line measurement cells or sampling approaches for zeolite characterization.

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