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@ARTICLE{Virtanen:860974,
author = {Virtanen, Otto L. J. and Kather, Michael and
Meyer-Kirschner, Julian and Melle, Andrea and Radulescu,
Aurel and Viell, Jörn and Mitsos, Alexander and Pich,
Andrij and Richtering, Walter},
title = {{D}irect {M}onitoring of {M}icrogel {F}ormation during
{P}recipitation {P}olymerization of {N}
-{I}sopropylacrylamide {U}sing in {S}itu {SANS}},
journal = {ACS omega},
volume = {4},
number = {2},
issn = {2470-1343},
address = {Washington, DC},
publisher = {ACS Publications},
reportid = {FZJ-2019-01607},
pages = {3690 - 3699},
year = {2019},
abstract = {Poly(N-isopropylacrylamide) microgels have found various
uses in fundamental polymer and colloid science as well as
in different applications. They are conveniently prepared by
precipitation polymerization. In this reaction, radical
polymerization and colloidal stabilization interact with
each other to produce well-defined thermosensitive particles
of narrow size distribution. However, the underlying
mechanism of precipitation polymerization has not been fully
understood. In particular, the crucial early stages of
microgel formation have been poorly investigated so far. In
this contribution, we have used small-angle neutron
scattering in conjunction with a stopped-flow device to
monitor the particle growth during precipitation
polymerization in situ. The average particle volume growth
is found to follow pseudo-first order kinetics, indicating
that the polymerization rate is determined by the
availability of the unreacted monomer, as the initiator
concentration does not change considerably during the
reaction. This is confirmed by calorimetric investigation of
the polymerization process. Peroxide initiator-induced
self-crosslinking of N-isopropylacrylamide and the use of
the bifunctional crosslinker N,N′-methylenebisacrylamide
are shown to decrease the particle number density in the
batch. The results of the in situ small-angle neutron
scattering measurements indicate that the particles form at
an early stage in the reaction and their number density
remains approximately the same thereafter. The overall
reaction rate is found to be sensitive to monomer and
initiator concentration in accordance with a radical
solution polymerization mechanism, supporting the results
from our earlier studies.},
cin = {JCNS-FRM-II / Neutronenstreuung ; JCNS-1 / IEK-10},
ddc = {660},
cid = {I:(DE-Juel1)JCNS-FRM-II-20110218 /
I:(DE-Juel1)JCNS-1-20110106 / I:(DE-Juel1)IEK-10-20170217},
pnm = {6G15 - FRM II / MLZ (POF3-6G15) / 6G4 - Jülich Centre for
Neutron Research (JCNS) (POF3-623)},
pid = {G:(DE-HGF)POF3-6G15 / G:(DE-HGF)POF3-6G4},
experiment = {EXP:(DE-MLZ)KWS2-20140101},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000460237300134},
doi = {10.1021/acsomega.8b03461},
url = {https://juser.fz-juelich.de/record/860974},
}