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@ARTICLE{Schiavone:1009542,
author = {Schiavone, Maria-Maddalena and Lamparelli, David Hermann
and Daniel, Christophe and Golla, Manuchar and Zhao, Yue and
Iwase, Hiroki and Arima-Osonoi, Hiroshi and Takata,
Shin-ichi and Szentmiklosi, Laszlo and Maroti, Boglarka and
Allgaier, Jürgen and Radulescu, Aurel},
title = {{E}xtended {Q} -range small-angle neutron scattering to
understand the morphology of proton-exchange membranes: the
case of the functionalized syndiotactic-polystyrene model
system},
journal = {Journal of applied crystallography},
volume = {56},
number = {4},
issn = {0021-8898},
address = {[Erscheinungsort nicht ermittelbar]},
publisher = {Wiley-Blackwell},
reportid = {FZJ-2023-02866},
pages = {947-960},
year = {2023},
abstract = {Semi-crystalline polymers exhibit microphase separation
into crystalline and amorphous domains characterized by
multiple structural levels with sizes ranging from
ångströms to hundreds of nanometres. The combination of
small-angle (SANS) and wide-angle (WANS) neutron scattering
on the same beamline enables reliable in situ
characterization of such materials under
application-relevant conditions, with the unique advantage
of contrast variation by controlled labelling, allowing the
structure of such multi-component systems to be resolved in
detail. This paper reports a structural analysis performed
on deuterated polymer membranes based on syndiotactic
polystyrene (sPS) using an extended Q-range SANS and WANS
combination, always with the same neutron scattering
instrument, either a pinhole SANS diffractometer installed
at a research reactor or a `small- and wide-angle'
time-of-flight diffractometer installed at a neutron
spallation source. sPS is a semi-crystalline material that
becomes hydrophilic and proton conducting when suitable
functionalization is achieved by thin film sulfonation, and
can form various co-crystalline complexes (clathrates) with
small organic molecules stored in the crystalline phase as
guests in the vacancies between the polymer helices.
Therefore, this material is interesting not only for its
conducting properties but also for its versatility as a
model system to evaluate the usefulness of extended Q-range
neutron scattering in such studies. Variation of neutron
contrast was achieved in the amorphous hydrophilic phase by
using H2O or D2O to hydrate the membranes and in the
crystalline phase by loading the clathrates with deuterated
or protonated guest molecules. The experimental approach,
the advantages and limitations of the two types of
instrumentation used in such analyses, and the main results
obtained with respect to the structural characterization of
sulfonated sPS membranes under different hydration and
temperature conditions are reported, and the potential of
this method for similar structural studies on other
semi-crystalline polymeric materials is discussed.},
cin = {JCNS-FRM-II / JCNS-1 / JCNS-4 / MLZ},
ddc = {540},
cid = {I:(DE-Juel1)JCNS-FRM-II-20110218 /
I:(DE-Juel1)JCNS-1-20110106 / I:(DE-Juel1)JCNS-4-20201012 /
I:(DE-588b)4597118-3},
pnm = {6G4 - Jülich Centre for Neutron Research (JCNS) (FZJ)
(POF4-6G4) / 632 - Materials – Quantum, Complex and
Functional Materials (POF4-632)},
pid = {G:(DE-HGF)POF4-6G4 / G:(DE-HGF)POF4-632},
experiment = {EXP:(DE-MLZ)KWS2-20140101},
typ = {PUB:(DE-HGF)16},
pubmed = {37555213},
UT = {WOS:001046279800004},
doi = {10.1107/S1600576723005496},
url = {https://juser.fz-juelich.de/record/1009542},
}