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@INPROCEEDINGS{Pienack:311595,
author = {Pienack, Nicole and Terraschke, Huayna and Bensch,
Wolfgang},
title = {{I}n-situ {C}rystallization {C}ell: {D}evelopments and
{F}irst {R}esults of the {M}odel {S}ystem ${A}l(acac)_{3}$},
reportid = {PUBDB-2016-04905},
year = {2016},
abstract = {In-situ investigations of the crystallization of solids are
still necessary for the understanding and the rational
synthesis of precursors, intermediates and products with
special or even improved properties.[1] With our
crystallization cell,[2] the detection and the control of
different reaction parameters during chemical reactions in
fluid media can be achieved. The modifications of the cell
allow in-situ experiments with X-ray diffraction (XRD).[2]
The crystallization of Al(acac)3 (acac = acetylacetonate) as
model system was investigated to demonstrate the performance
of the cell. First in-situ energy-dispersive X-ray
diffraction (EDXRD) experiments were carried out at the
beamline F3 (DORIS, DESY). During the crystallization of
Al(acac)3 changes of pH value and redox potential could be
observed, but a higher concentrated reaction suspension was
required for obtaining suitable EDXRD spectra. In subsequent
in-situ XRD experiments at beamline P07B (PETRA III, DESY)
with modified reaction vessels in a special sample holder
(Fig. 1) the growth of the Bragg peaks during the
crystallization of Al(acac)3 could be detected. The
possibility of integrating further methods and/or sensors is
highly important while working with synchrotron radiation
(Fig. 1). Hence, the potential of the cell was proved to be
beneficial for controlling and monitoring several reaction
parameters during the crystallization.},
month = {Sep},
date = {2016-09-19},
organization = {18. Conference of the GDCh Division
Solid State Chemistry and Materials
Research, Innsbruck (Austria), 19 Sep
2016 - 21 Sep 2016},
cin = {DOOR},
cid = {I:(DE-H253)HAS-User-20120731},
pnm = {6G3 - PETRA III (POF3-622)},
pid = {G:(DE-HGF)POF3-6G3},
experiment = {EXP:(DE-H253)D-F3-20150101 / EXP:(DE-H253)P-P07-20150101 /
EXP:(DE-H253)P-P09-20150101},
typ = {PUB:(DE-HGF)1},
url = {https://bib-pubdb1.desy.de/record/311595},
}