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Concept for a Time-of-Flight Small Angle Neutron Scattering Instrument at the European Spallation Source
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A new Small Angle Neutron Scattering instrument is proposed for the European Spallation Source. The pulsed source requires a time-of-flight analysis of the gathered neutrons at the detector. The optimal instrument length is found to be rather large, which allows for a polarizer and a versatile collimation. The polarizer allows for studying magnetic samples and incoherent background subtraction. The wide collimation will host VSANS and SESANS options that increase the resolution of the instrument towards um and tens of um, respectively. Two 1m2 area detectors will cover a large solid angle simultaneously. The expected gains for this new instrument will lie in the range between 20 and 36, depending on the assessment criteria, when compared to up-to-date reactor based instruments. This will open new perspectives for fast kinetics, weakly scattering samples, and multi-dimensional contrast variation studies
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Physical Review E
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Close to a planar surface, lamellar structures are imposed upon otherwise bulk bicontinuous microemulsions. Thermally induced membrane undulations are modified by the presence of the rigid interface. While it has been shown that a pure membrane's dynamics are accelerated close to the interface, we observed nearly unchanged relaxation rates for membranes spiked with large amphiphilic diblock copolymers. An increase of the polymer concentration by a factor of 2–3 for the first and second surfactant membrane layers was observed. We interpret the reduced relaxation times as the result of an interplay between the bending rigidity and the characteristic distance of the first surfactant membrane to the rigid interface, which causes the hydrodynamic and steric interface effects described in Seifert's theory. The influence of these effects on decorated membranes yields a reduction of the frequencies and an amplification of the amplitudes of long-wavelength undulations, which are in accordance to our experimental findings
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Polymer enrichment decelerates surfactant membranes near interfaces
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10.1016/j.ijmultiphaseflow.2013.04.004
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Crossref
10.1016/j.petrol.2009.01.009
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Crossref
10.1140/epje/i2001-10112-9
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C. Cottin-Bizonne
47 -
Crossref
Eur. Phys. J. E
9
2002
10.1103/PhysRevLett.103.248302
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Crossref
10.1103/PhysRevLett.82.4671
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10.1140/epjst/e2007-00024-0
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10.1103/PhysRevE.83.030401
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10.1103/PhysRevE.85.041408
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10.1051/epjconf/20123303005
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10.1103/PhysRevE.66.041504
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Crossref
10.1063/1.1857523
-- missing cx lookup --
Crossref
J. Allgaier
2009
Crossref
Microemulsions
J. Allgaier Microemulsions 2009
10.1016/S0168-9002(97)00956-X
-- missing cx lookup --
Crossref
10.1088/0957-0233/19/3/034022
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Crossref
10.1016/j.nima.2012.08.059
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Crossref
10.1103/PhysRevLett.77.4788
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Crossref
10.1051/jp2:1994191
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Crossref
10.1103/PhysRevE.49.3124
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Crossref
10.1016/S0301-0104(02)00548-7
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Crossref
10.1209/0295-5075/9/1/011
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Crossref
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Bras, Ana
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Krutyeva, M.
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fzj
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Sharp, M.
3
P:(DE-HGF)0
Falus, P.
4
P:(DE-Juel1)144382
Feoktystov, A.
5
fzj
P:(DE-HGF)0
Gasser, U.
6
P:(DE-Juel1)130902
Pyckhout-Hintzen, W.
7
fzj
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Wischnewski, A.
8
fzj
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Richter, D.
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fzj
FZJ-2014-05270
EXP:(DE-MLZ)KWS1-20140101
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EXP:(DE-MLZ)KWS1-20140101
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Forschungs-Neutronenquelle Heinz Maier-Leibnitz
KWS-1: Small angle scattering diffractometer
NL3b
0
h.lexis@fz-juelich.de
http://juser.fz-juelich.de/record/171701/files/FZJ-2014-05270.pdf
OpenAccess
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2014-09-05
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2014-08-29
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oai:juser.fz-juelich.de:171701
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We present neutron scattering data on the structure and dynamics of melts from polyethylene oxide rings with molecular weights up to ten times the entanglement mass of the linear counterpart. The data reveal a very compact conformation displaying a structure approaching a mass fractal, as hypothesized by recent simulation work. The dynamics is characterized by a fast Rouse relaxation of subunits (loops) and a slower dynamics displaying a lattice animal-like loop displacement. The loop size is an intrinsic property of the ring architecture and is independent of molecular weight. This is the first experimental observation of the space-time evolution of segmental motion in ring polymers illustrating the dynamic consequences of their topology that is unique among all polymeric systems of any other known architecture.
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FZJ
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G:(DE-HGF)POF3-550
G:(DE-HGF)POF3-500
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Von Materie zu Materialien und Leben
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PERI:(DE-600)1472655-5
10.1103/PhysRevLett.113.168302
Vol. 113, no. 16, p. 168302
16
168302
Physical review letters
113
1079-7114
2014
550
Dataset connected to CrossRef, juser.fz-juelich.de
Molecular Scale Dynamics of Large Ring Polymers
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10.1103/PhysRevLett.113.168302
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0031-9007
ISSN
1079-7114
Handle
2128/8025
WOS
WOS:000344032500011
College Park, Md.
APS
2014
P:(DE-Juel1)144649
Goossen, Sebastian
0
Corresponding Author
fzj
h.lexis@fz-juelich.de
2015-02-02T13:45:39.154334
2014-10-20T14:41:33.143382
2014-10-20T14:41:33.143382
2015-02-02T13:45:39.154334
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ICS-1
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JCNS (München) ; Jülich Centre for Neutron Science JCNS (München) ; JCNS-FRM-II
JCNS-FRM-II
1
I:(DE-Juel1)JCNS-1-20110106
Neutronenstreuung ; JCNS-1
Neutronenstreuung
2
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1423054171_20929
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P:(DE-Juel1)130509
Arend, N.
1
fzj
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Lunkenheimer, P.
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Loidl, A.
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P:(DE-Juel1)129542
Stingaciu, L.
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fzj
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Jalarvo, N.
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fzj
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Mamontov, E.
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P:(DE-Juel1)130872
Ohl, M.
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fzj
FZJ-2015-01260
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EXP:(DE-Juel1)SNS-NSE-20150203
SNS-NSE: Neutron Spin Echo Spectrometer
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h.lexis@fz-juelich.de
http://juser.fz-juelich.de/record/187634/files/FZJ-2015-01260.pdf
OpenAccess
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Hybrid-OA
2016-02-06
Zahlung erfolgt
2015-01-30
65200/E2310525
Hybrid-OA über KST 65200 ; Proj. E2310525
oai:juser.fz-juelich.de:187634
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The relaxational dynamics in glass-forming glycerol and glycerol mixed with LiCl is investigated using different neutron scattering techniques. The performed neutron spin echo experiments, which extend up to relatively long relaxation time scales of the order of 10ns, should allow for the detection of contributions from the so-called excess wing. This phenomenon, whose microscopic origin is controversially discussed, arises in a variety of glass formers and, until now, was almost exclusively investigated by dielectric spectroscopy and light scattering. Here we show that the relaxational process causing the excess wing can also be detected by neutron scattering, which directly couples to density fluctuations
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PERI:(DE-600)2004003-9
10.1140/epje/i2015-15001-0
Vol. 38, no. 1, p. 1
1
1
The @European physical journal / E
38
1292-895X
2015
530
Dataset connected to CrossRef, juser.fz-juelich.de
Excess wing in glass-forming glycerol and LiCl-glycerol mixtures detected by neutron scattering
doi
10.1140/epje/i2015-15001-0
ISSN
1292-8941
ISSN
1292-895X
Handle
2128/8373
WOS
WOS:000348567400001
Berlin
Springer
2015
P:(DE-Juel1)130679
Gupta, S.
0
Corresponding Author
fzj
h.lexis@fz-juelich.de
2015-02-04T13:49:52.899617
2015-02-02T08:11:18.809444
2015-02-02T08:11:18.809444
2015-02-04T13:49:52.899617
I:(DE-Juel1)ICS-1-20110106
ICS-1
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0
I:(DE-Juel1)JCNS-FRM-II-20110218
JCNS (München) ; Jülich Centre for Neutron Science JCNS (München) ; JCNS-FRM-II
JCNS-FRM-II
1
I:(DE-Juel1)JCNS-1-20110106
Neutronenstreuung ; JCNS-1
Neutronenstreuung
2
I:(DE-Juel1)JCNS-SNS-20110128
JCNS-SNS
JCNS-SNS
3
oai:juser.fz-juelich.de:187634
oai:juser.fz-juelich.de:1882132022-10-01T09:34:48ZopenCostOpenAPCVDBVDB:MLZ
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10.1016/j.polymer.2015.01.039
doi
0032-3861
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1873-2291
ISSN
WOS:000351117300021
WOS
FZJ-2015-01655
540
Campanella, A.
P:(DE-Juel1)157777
0
Corresponding Author
fzj
Nanocomposites composed of HEUR polymer and magnetite iron oxide nanoparticles: Structure and magnetic response of the hydrogel and dried state
Oxford
2015
Elsevier Science
Journal Article
journal
journal
PUB:(DE-HGF)16
1425372095_24704
PUB:(DE-HGF)
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A novel nanocomposite system composed of hydrophobically modified ethoxylated urethane (so-called HEUR) polymer, which is a telechelic polymer, and coated magnetite (Fe3O4) nanoparticles (MNp) is investigated. Two different kinds of nanoparticle coatings, are used: a hydrophobic coating composed of oleic acid and oleylamine and a hydrophilic coating having the cationic surfactant C18TAB as an additional layer to the hydrophobic nanoparticles. The structure of the nanocomposites as hydrogels with either MNp separately is analyzed using small angle neutron scattering (SANS). Furthermore, the dried state is studied in complementary SANS experiments. The magnetic response of the dried state is characterized by magnometry observing a superparamagnetic behavior.
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Nano Science and Technology
V:(DE-MLZ)GC-150
V:(DE-HGF)
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Forschungs-Neutronenquelle Heinz Maier-Leibnitz
KWS-1: Small angle scattering diffractometer
NL3b
EXP:(DE-MLZ)FRMII-20140101
EXP:(DE-MLZ)KWS1-20140101
EXP:(DE-MLZ)KWS1-20140101
EXP:(DE-MLZ)NL3b-20140101
0
Di, Z.
P:(DE-Juel1)141663
1
fzj
Luchini, A.
P:(DE-HGF)0
2
Paduano, L.
P:(DE-HGF)0
3
Klapper, A.
P:(DE-Juel1)144041
4
fzj
Herlitschke, M.
P:(DE-Juel1)145213
5
fzj
Petracic, O.
P:(DE-Juel1)145895
6
fzj
Appavou, M. S.
P:(DE-Juel1)130507
7
fzj
Müller-Buschbaum, P.
P:(DE-HGF)0
8
Frielinghaus, H.
P:(DE-Juel1)130646
9
fzj
Richter, D.
P:(DE-Juel1)130917
10
fzj
10.1016/j.polymer.2015.01.039
Vol. 60, p. 176 - 185
PERI:(DE-600)2013972-X
176 - 185
Polymer
60
2015
0032-3861
h.lexis@fz-juelich.de
http://juser.fz-juelich.de/record/188213/files/FZJ-2015-01655.pdf
Restricted
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Colour charges
2015-03-09
Zahlung erfolgt
2015-03-04
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oai:juser.fz-juelich.de:188213
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Von Materie zu Materialien und Leben
G:(DE-HGF)POF3-620
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A basic understanding of biological membranes is of paramount importance as these membranes comprise the very building blocks of life itself. Cells depend in their function on a range of properties of the membrane, which are important for the stability and function of the cell, information and nutrient transport, waste disposal, and finally the admission of drugs into the cell and also the deflection of bacteria and viruses. We have investigated the influence of ibuprofen on the structure and dynamics of L-α-phosphatidylcholine (SoyPC) membranes by means of grazing incidence small-angle neutron scattering, neutron reflectometry, and grazing incidence neutron spin echo spectroscopy. From the results of these experiments, we were able to determine that ibuprofen induces a two-step structuring behavior in the SoyPC films, where the structure evolves from the purely lamellar phase for pure SoyPC over a superposition of two hexagonal phases to a purely hexagonal phase at high concentrations. A relaxation, which is visible when no ibuprofen is present in the membrane, vanishes upon addition of ibuprofen. This we attribute to a stiffening of the membrane. This behavior may be instrumental in explaining the toxic behavior of ibuprofen in long-term application.
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2000
Crossref
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Crossref
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We investigate the dynamics of kinetically frozen block copolymer micelles of different softness across a wide range of particle concentrations, from the fluid to the onset of glassy behavior, through a combination of rheology, dynamic light scattering, and pulsed field gradient NMR spectroscopy. We additionally perform Brownian dynamics simulations based on an ultrasoft coarse-grained potential, which are found to be in quantitative agreement with experiments, capturing even the very details of dynamic structure factors S(Q,t) on approaching the glass transition. We provide evidence that for these systems the Stokes-Einstein relation holds up to the glass transition; given that it is violated for dense suspensions of hard colloids, our findings suggest that its validity is an intriguing signature of ultrasoft interactions.
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Goossen, Sebastian
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Sensing Polymer Chain Dynamics through Ring Topology: A Neutron Spin Echo Study
College Park, Md.
2015
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Using neutron spin echo spectroscopy, we show that the segmental dynamics of polymer rings immersed in linear chains is completely controlled by the host. This transforms rings into ideal probes for studying the entanglement dynamics of the embedding matrix. As a consequence of the unique ring topology, in long chain matrices the entanglement spacing is directly revealed, unaffected by local reptation of the host molecules beyond this distance. In shorter entangled matrices, where in the time frame of the experiment secondary effects such as contour length fluctuations or constraint release could play a role, the ring motion reveals that the contour length fluctuation is weaker than assumed in state-of-the-art rheology and that the constraint release is negligible. We expect that rings, as topological probes, will also grant direct access to molecular aspects of polymer motion which have been inaccessible until now within chains adhering to more complex architectures.
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10.1103/PhysRevLett.115.148302
Vol. 115, no. 14, p. 148302
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148302
Physical review letters
115
2015
1079-7114
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Radulescu, Aurel
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Morphology of crystalline–amorphous olefin block copolymers in solution characterized by small-angle neutron scattering and microscopy
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2015
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The single-chain properties and self-assembly behavior in dilute solution of olefin block copolymers obtained by chain-shuttling technology and consisting of alternating crystallizable and amorphous ethylene/1-octene blocks were investigated by pinhole and focusing small-angle neutron scattering techniques, optical microscopy in bright-field and crossed-polarizer modes, and differential scanning calorimetry. The complex hydrocarbon soluble (precipitant free) macro-aggregates formed with decreasing temperature are characterized by spherulitic textures. The spherulites yield, on one hand, a morphology that depends on the chain structure properties and, on the other hand, multiple structural levels with a hierarchical organization that ranges from 10 Å up to tens of micrometres. This morphology displays peculiarities dictated by the polydisperse character of these materials.
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Tuning the instrument resolution using chopper and time of flight at the small-angle neutron scattering diffractometer KWS-2
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Munksgaard
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Following demand from the user community regarding the possibility of improving the experimental resolution, the dedicated high-intensity/extended Q-range SANS diffractometer KWS-2 of the Jülich Centre for Neutron Science at the Heinz Maier-Leibnitz Center in Garching was equipped with a double-disc chopper with a variable opening slit window and time-of-flight (TOF) data acquisition option. The chopper used in concert with a dedicated high-intensity velocity selector enables the tuning at will of the wavelength resolution [Delta][lambda]/[lambda] within a broad range, from 20% (standard) down to 2%, in a convenient and safe manner following pre-planned or spontaneous decisions during the experiment. The new working mode is described in detail, and its efficiency is demonstrated on several standard samples with known properties and on a completely new crystallizable copolymer system, which were investigated using both the conventional (static) and TOF modes.
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Photoactivation Reduces Side-Chain Dynamics of a LOV Photoreceptor
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We used neutron-scattering experiments to probe the conformational dynamics of the light, oxygen, voltage (LOV) photoreceptor PpSB1-LOV from Pseudomonas putida in both the dark and light states. Global protein diffusion and internal macromolecular dynamics were measured using incoherent neutron time-of-flight and backscattering spectroscopy on the picosecond to nanosecond timescales. Global protein diffusion of PpSB1-LOV is not influenced by photoactivation. Observation-time-dependent global diffusion coefficients were found, which converge on the nanosecond timescale toward diffusion coefficients determined by dynamic light scattering. Mean-square displacements of localized internal motions and effective force constants, <k′>, describing the resilience of the proteins were determined on the respective timescales. Photoactivation significantly modifies the flexibility and the resilience of PpSB1-LOV. On the fast, picosecond timescale, small changes in the mean-square displacement and <k′> are observed, which are enhanced on the slower, nanosecond timescale. Photoactivation results in a slightly larger resilience of the photoreceptor on the fast, picosecond timescale, whereas in the nanosecond range, a significantly less resilient structure of the light-state protein is observed. For a residue-resolved interpretation of the experimental neutron-scattering data, we analyzed molecular dynamics simulations of the PpSB1-LOV X-ray structure. Based on these data, it is tempting to speculate that light-induced changes in the protein result in altered side-chain mobility mostly for residues on the protruding Jα helix and on the LOV-LOV dimer interface. Our results provide strong experimental evidence that side-chain dynamics play a crucial role in photoactivation and signaling of PpSB1-LOV via modulation of conformational entropy.
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A flexible linker region between three fragments allows antibodies to adjust their binding sites to an antigen or receptor. Using Neutron Spin Echo Spectroscopy we observed fragment motion on a timescale of 7 ns with motional amplitudes of about 1 nm relative to each other. The mechanistic complexity of the linker region can be described by a spring model with Brownian motion of the fragments in a harmonic potential. Displacements, timescale, friction and force constant of the underlying dynamics are accessed. The force constant exhibits a similar strength to an entropic spring, with friction of the fragment matching the unbound state. The observed fast motions are fluctuations in pre-existing equilibrium configurations. The Brownian motion of domains in a harmonic potential is the appropriate model to examine functional hinge motions dependent on the structural topology and highlights the role of internal forces and friction to function.
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Zhang-Haagen, Bo
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2016
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Small proteins like amyloid beta (Aβ) monomers are related to neurodegenerative disorders by aggregation to insoluble fibrils. Small angle neutron scattering (SANS) is a nondestructive method to observe the aggregation process in solution. We show that SANS is able to resolve monomers of small molecular weight like Aβ for aggregation studies. We examine Aβ monomers after prolonged storing in d-hexafluoroisopropanol (dHFIP) by using SANS and dynamic light scattering (DLS). We determined the radius of gyration from SANS as 1.0±0.1 nm for Aβ1–40 and 1.6±0.1 nm for Aβ1–42 in agreement with 3D NMR structures in similar solvents suggesting a solvent surface layer with 5% increased density. After initial dissolution in dHFIP Aβ aggregates sediment with a major component of pure monomers showing a hydrodynamic radius of 1.8±0.3 nm for Aβ1–40 and 3.2±0.4 nm for Aβ1–42 including a surface layer of dHFIP solvent molecules.
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2016
1932-6203
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Dielectric relaxations of nanocomposites composed of HEUR polymers and magnetite nanoparticles
Oxford
2016
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We investigate the dynamics of nanocomposites composed of hydrophobically modified ethoxylated urethanes (HEUR) and magnetite nanoparticles (MNPs) as dry films. Weemployed dielectric relaxation spectroscopy (DRS) in combination with differential scanning calorimetry (DSC) and thermally stimulated depolarization currents (TSDC).The three techniques reveal a strong heterogeneity of the matrix of the nanocomposites, consisting of (i) a crystalline poly(ethyleneoxide) PEO bulk phase, (ii) an amorphous PEO portion, and (iii) small PEO crystallites which experience different constraints than the PEO bulk phase. TSDC and DRS reveal a very high direct current (DC)-conductivity of the pure matrix, which increases with MNPs concentration. The increase of the DCconductivity is not related to an increase of the segmental mobility, but most likely to the change of the morphology of the hydrophobic domains of the polymer matrix, due to the formation of large MNPs clusters. Indeed, the MNPs neither influence the segmental dynamics of the polymer nor the phase behavior of the polymer matrix. The addition of MNPs slightly increases the activation energy related to the γ-relaxation of the polymer. This effect might be related to the changes in nano-morphology as demonstrated by the slight increase of the degree of crystallinity. The analysis of the DRS data with the electrical modulus M’’(ω) and the derivative ε’’der formalism allow us to identify a low-frequency process in addition to the conductivity relaxation. This low-frequency dispersion is also revealed by TSDC. It is most likely related to the Maxwell-Wagner- Sillars relaxation, which typically occurs in systems which feature phase separation. The detailed investigation of the dielectric properties of these novel nanocomposites with increasing MNPs concentration will be useful for their practical application, for example as absorbers of electromagnetic waves.
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Frozen O$_{2}$ layer revealed by neutron reflectometry
Amsterdam [u.a.]
2016
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A 63 Å thick film originating from frozen air on a solid substrate has been investigated via neutron reflectometry. The experiment shows that neutron reflectometry allows performing chemical surface analysis by quantifying the composition of this frozen layer and identifies the film to be frozen oxygen
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570
Sill, Clemens
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Structure and domain dynamics of human lactoferrin in solution and the influence of Fe(III)-ion ligand binding
London
2016
BioMed Central
article
DRIVER
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1484916656_27106
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BackgroundHuman lactoferrin is an iron-binding protein of the innate immune system consisting of two connected lobes, each with a binding site located in a cleft. The clefts in each lobe undergo a hinge movement from open to close when Fe3+ is present in the solution and can be bound. The binding mechanism was assumed to relate on thermal domain fluctuations of the cleft domains prior to binding. We used Small Angle Neutron Scattering and Neutron Spin Echo Spectroscopy to determine the lactoferrin structure and domain dynamics in solution.ResultsWhen Fe3+ is present in solution interparticle interactions change from repulsive to attractive in conjunction with emerging metas aggregates, which are not observed without Fe3+. The protein form factor shows the expected change due to lobe closing if Fe3+ is present. The dominating motions of internal domain dynamics with relaxation times in the 30–50 ns range show strong bending and stretching modes with a steric suppressed torsion, but are almost independent of the cleft conformation. Thermally driven cleft closing motions of relevant amplitude are not observed if the cleft is open.ConclusionThe Fe3+ binding mechanism is not related to thermal equilibrium fluctuations closing the cleft. A likely explanation may be that upon entering the cleft the iron ion first binds weakly which destabilizes and softens the hinge region and enables large fluctuations that then close the cleft resulting in the final formation of the stable iron binding site and, at the same time, stable closed conformation.
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2016
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A new dual network elastomer is developed that consists of polybutadiene crosslinked with both permanent and transient bonds. The transient network is formed by the association of urazole groups that are randomly attached to the polymer backbone. Subsequent orthogonal covalent crosslinking through hydrosilylation in the melt state leads to a dual network with variable permanent and transient crosslinking density. Small angle neutron scattering (SANS) investigations show a homogeneous distribution of the transient bonds in both the functionalized polymers and the dual network products. The enhanced mechanical properties of the dual networks compared to conventional polybutadiene elastomers are characterized by stress–strain measurements. The increased toughness can be explained by a protective mechanism where the weaker supramolecular bonds act as sacrificial bonds that dissipate energy
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We have studied the motion of polyhedral oligomeric silsesquioxane (POSS) nanoparticles modified with poly(ethylene glycol) (PEG) arms immersed in PEG matrices of different molecular weight. Employing neutron spin echo spectroscopy in combination with pulsed field gradient (PFG) NMR we found the following. (i) For entangled matrices the center of mass mean square displacement (MSD) of the PEG-POSS particles is subdiffusive following a t0.56 power law. (ii) The diffusion coefficient as well as the crossover to Fickian diffusion is independent of the matrix molecular weight and takes place as soon as the center of mass has moved a distance corresponding to the particle radius—this holds also for unentangled hosts. (iii) For the entangled matrices Rubinstein’s scaling theory is validated; however, the numbers indicate that beyond Rouse friction the entanglement constraints appear to strongly increase the effective friction even on the nanoparticle length scale imposing a caveat on the interpretation of microrheological experiments. (iv) The oligomer decorated PEG-POSS particles exhibit the dynamics of a Gaussian star with an internal viscosity that rises with an increase of the host molecular weight.
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HERITAGE: the concept of a giant flux neutron reflectometer for the exploration of 3-d structure of free-liquid and solid interfaces in thin films
Amsterdam
2017
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The instrumental concept of HERITAGE – a reflectometer with a horizontal sample geometry – well fitted to the long pulse structure of a neutron source is presented. It is constitutes a new class of reflectometers achieving the unprecedentedly high flux for classical specular reflectometry combined with off-specular reflectometry and grazing incidence small-angle scattering (GISANS), thus resulting in a complete 3-d exploration of lateral and in depth structures in thin films. This is achieved by specially designed neutron guides. In the horizontal direction (perpendicular to the scattering plane) the guide's elliptic shape focusses the neutrons onto the sample. In the vertical direction a multichannel geometry provides a smooth divergence distribution at the sample position while accepting the entire beam from a compact high-brilliance flat moderator.The modular collimation setup of HERITAGE provides extremely high flexibility in respect to sample geometries and environments, including the possibility to study virtually all types of solid and liquid interfaces, statically or kinetically. The use of multiple beam illumination allows for reflectivity and GISANS measurements at liquid interfaces both from above and below without a need to move the sample.This concept assures the delivery of the maximum possible and usable flux to the sample in both reflectivity and GISANS measurement regimes. The presented design outperforms the flux of all present-day and already for the ESS planned reflectometers and GISANS setups in flux and in measuring time for standard samples.
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Mark, C.
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Polymer Chain Conformation and Dynamical Confinement in a Model One-Component Nanocomposite
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We report a neutron-scattering investigation on the structure and dynamics of a single-component nanocomposite based on SiO2 particles that were grafted with polyisoprene chains at the entanglement limit. By skillful labeling, we access both the monomer density in the corona as well as the conformation of the grafted chains. While the corona profile follows a r−1 power law, the conformation of a grafted chain is identical to that of a chain in a reference melt, implying a high mutual penetration of the coronas from different particles. The brush crowding leads to topological confinement of the chain dynamics: (i) At local scales, the segmental dynamics is unchanged compared to the reference melt, while (ii) at the scale of the chain, the dynamics appears to be slowed down; (iii) by performing a mode analysis in terms of end-fixed Rouse chains, the slower dynamics is tracked to topological confinement within the cone spanned by the adjacent grafts; (iv) by adding 50% matrix chains, the topological confinement sensed by the grafted chain is lifted partially and the apparent chain motion is accelerated. We observe a crossover from pure Rouse motion at short times to topological confined motion beyond the time when the segmental mean squared displacement has reached the distance to the next graft.
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10.1103/PhysRevLett.119.047801
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New tools for grazing incidence neutron scattering experiments open perspectives to study nano-scale tribology mechanisms
Amsterdam
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Using grazing incidence scattering methods allows for depth profiling near surface structures very efficiently Dosch (1986). In parallel, layered structures have been used as resonators to enhance the wave field Kozhevnikov et al. (2007), Khaydukov et al. (2011), Kozhevnikov et al. (2011) and Nesnidal and Walker (1996) that directly increases the scattered intensity too. Third, the combination of these methods with neutron spin echo spectroscopy allows for near surface studies of dynamics Jaksch et al. (2015) and Frielinghaus et al. (2012) that can be correlated to tribological effects on the molecular level. This field of science, the tribology, - so far - has been driven mainly by the surface force balance that measures the macroscopic response of the system (latest research employs also AFM) Raviv et al. (2003) [1], Chung et al. (2016) [2] and Mocny and Klok (2016) [3]. The progress of this method was to reach the nano-scale distances that were necessary to obtain information about the friction of the nano-structures. The proposed method of grazing incidence neutron spin echo spectroscopy gives access to much more detailed information of molecular response to confinement by one or two hard walls, and therefore would pave the way for very rich and precise tribological comparisons of theory with experiments.
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Sun, J.-P.
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Hydrostatic pressure effects on the static magnetism in Eu(Fe$_{0.925}$Co$_{0.075}$)$_{2}$As$_{2}$
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2017
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EuFe2As2-based iron pnictides are quite interesting compounds, due to the two magnetic sublattices in them and the tunability to superconductors by chemical doping or application of external pressure. The effects of hydrostatic pressure on the static magnetism in Eu(Fe0.925Co0.075)2As2 are investigated by complementary electrical resistivity, ac magnetic susceptibility and single-crystal neutron diffraction measurements. A specific pressure-temperature (P-T) phase diagram of Eu(Fe0.925Co0.075)2As2 is established. The structural phase transition, as well as the spin-density-wave order of Fe sublattice, is suppressed gradually with increasing pressure and disappears completely above 2.0 GPa. In contrast, the magnetic order of Eu sublattice persists over the whole investigated pressure range up to 14 GPa, yet displaying a non-monotonic variation with pressure. With the increase of the hydrostatic pressure, the magnetic state of Eu evolves from the canted antiferromagnetic structure in the ground state, via a pure ferromagnetic structure under the intermediate pressure, finally to an “unconfirmed” antiferromagnetic structure under the high pressure. The strong ferromagnetism of Eu coexists with the pressure-induced superconductivity around 2 GPa. Comparisons between the P-T phase diagrams of Eu(Fe0.925Co0.075)2As2 and the parent compound EuFe2As2 were also made.
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000
Jaksch, Sebastian
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fzj
Nanoscale rheology at solid-complex fluid interfaces
London
2017
Nature Publishing Group
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Here we present an approach to measure dynamic membrane properties of phospholipid membranes close to an interface. As an example we show results of the membrane dynamics of a phospholipid membrane multilayer-stack on a solid substrate (silicon). On this sample we were able to measure local interaction and friction parameters using Grazing Incidence Neutron Spin Echo Spectroscopy (GINSES), where an evanescent neutron wave probes the fluctuations close to a rigid interface. With this method it is possible to access length scales in the nano to micrometer region as well as energies in the μeV range. Using a new neutron resonator structure we achieved the required intensity gain for this experiment. During our investigations we found an excitation mode of the phospholipid membrane that has not been reported previously and only became visible using the new methodology. We speculate that the energy transported by that undulation can also serve to distribute energy over a larger area of the membrane, stabilizing it. This new methodology has the capability to probe the viscoelastic effects of biological membranes, becoming a new tool for tribology on the nanoscale and has allowed the observation of the hitherto invisible property of phospholipid membranes using neutrons.
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4417
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7
2017
2045-2322
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http://juser.fz-juelich.de/record/837317/files/Jaksch_SREP2017.pdf
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20221001113500.0
10.1039/C7NR06169B
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2040-3364
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WOS:000415666500041
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FZJ-2017-07419
English
600
Houston, Judith E.
P:(DE-Juel1)171614
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A self-assembly toolbox for thiophene-based conjugated polyelectrolytes: surfactants, solvent and copolymerisation
Cambridge
2017
RSC Publ.
article
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Targeted control of the aggregation, morphology and optical properties of conjugated polymers is critical for the development of high performance optoelectronic devices. Here, self-assembly approaches are used to strategically manipulate the order, conformation and spatial distribution of conjugated polymers in solution and subsequently prepared thin films. The supramolecular complex organisation of phosphonium-functionalised homo- (P3HTPMe3) and diblock (P3HT-b-P3HTPMe3) ionic conjugated polythiophenes upon solvent-mediation and co-assembly with oppositely charged surfactants is investigated. UV/Vis absorption and photoluminescence spectroscopies, small-angle neutron scattering (SANS), cryo-transmission electron microscopy (cryo-TEM) and atomic force microscopy (AFM) are used to probe the organisation and photophysical response of the aggregates formed. Subtle differences in the surfactant mole fraction and structure, as well as the solvent polarity, yield differences in the nature of the resultant homopolyelectrolyte-surfactant complexes. In contrast, only moderate structural transformations are observed for the amphiphilic diblock copolyelectrolyte, emphasising the structure “anchoring” effect of a neutral polymer block when amphiphilic copolymers are dissolved in polar solvents. These results highlight the versatility of self-assembly to access a range of nanomorphologies, which could be crucial for the design of the next generation of organic optoelectronic devices.
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Evans, Rachel C.
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10.1039/C7NR06169B
p. 10.1039.C7NR06169B
PERI:(DE-600)2515664-0
44
17481-17493
Nanoscale
9
2017
2040-3372
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http://juser.fz-juelich.de/record/838913/files/SL33095%20C17052.pdf
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10.1016/j.nima.2017.11.085
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2128/16348
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altmetric:30548241
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FZJ-2018-00064
530
Voigt, J.
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Spectrometers for compact neutron sources
Amsterdam
2018
North-Holland Publ. Co.
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PUB:(DE-HGF)16
1553872259_28546
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We discuss the potential for neutron spectrometers at novel accelerator driven compact neutron sources. Such a High Brilliance Source (HBS) relies on low energy nuclear reactions, which enable cryogenic moderators in very close proximity to the target and neutron optics at comparably short distances from the moderator compared to existing sources. While the first effect aims at increasing the phase space density of a moderator, the second allows the extraction of a large phase space volume, which is typically requested for spectrometer applications. We find that competitive spectrometers can be realized if (a) the neutron production rate can be synchronized with the experiment repetition rate and (b) the emission characteristics of the moderator can be matched to the phase space requirements of the experiment. MCNP simulations for protons or deuterons on a Beryllium target with a suitable target/moderator design yield a source brightness, from which we calculate the sample fluxes by phase space considerations for different types of spectrometers. These match closely the figures of todays spectrometers at medium flux sources. Hence we conclude that compact neutron sources might be a viable option for next generation neutron sources
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10.1016/j.nima.2017.11.085
Vol. 884, p. 59 - 63
PERI:(DE-600)1466532-3
59 - 63
Nuclear instruments & methods in physics research / A
884
2018
0168-9002
connie.hesse@frm2.tum.de
http://juser.fz-juelich.de/record/841760/files/1-s2.0-S0168900217313414-main.pdf
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Mangiapia, Gaetano
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Effect of Benzocaine and Propranolol on phospholipid-based bilayers
Cambridge
2017
RSC Publ.
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Cell membranes play a fundamental role in protecting the cell from its surroundings, in addition to host many proteins with fundamental biological tasks. A study of drug/lipid interactions is a necessary and important step to fully clarify the role and action mechanism of active ingredients, as well as to shed light on possible complications caused by drug overdosage. In this paper, the influence of Benzocaine and Propranolol drugs on the structure of L-α-phosphatidylcholines-based membranes has been investigated by means of neutron reflectivity, grazing incidence small angle neutron scattering, and small/ultrasmall angle neutron scattering. Investigations allowed discovering a stiffening of the membranes as well as the formation of stalks, caused by the presence of Benzocaine. On the other hand, disordered bilayers (lamellar powders) and highly curved structures were found in the presence of Propranolol. The found results may be rationalized in terms of the molecular structure of drugs and may serve as starting point for explaining the toxic behavior in long-term and overdosage scenarios.
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Schiavone, Maria Maddalena
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Structure and morphology of model polymer electrolyte membranes based on sulfonated syndiotactic-polystyrene in the δ co-crystalline phase resolved by small-angle neutron scattering
Amsterdam [u.a.]
2018
Elsevier Science
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Syndiotactic polystyrene (s-PS) is able to form different kinds of co-crystalline phases with guest molecules of different size, shape and property. Several advanced materials have been produced starting from s-PS co-crystalline films. In particular, sulfonated s-PS (s-sPS) can be used as proton-conductive membrane in some fuel cells applications, as it presents high proton conductivity (comparable with Nafion). Besides, it shows a high chemical and thermo-mechanical stability and a low cost. The morphology of different s-PS clathrates and the structural behavior of s-sPS upon hydration can be thoroughly understood by SANS. In fact, exploiting the neutron contrast variation between various hydrogenated and deuterated components of s-PS and s-sPS clathrates, additional and unique information about the distribution of guest molecules in the crystalline and amorphous regions and about the hydrated domains of the polymer were obtained. Moreover, using uni-axially deformed films the occurrence and distribution of scattering features from typical morphologies on specific directions and sectors of detection plan enable an accurate structural study of such complex polymeric systems. We report in the present paper a detailed SANS investigation of s-PS films, starting from their crystallization with guest molecules to the subsequent sulfonation and hydration. FT-IR, neutron PGAA, WAXD and cryo-TEM were used complementary to SANS to check the state of the samples after each step of the treatment process and to obtain additional structural information as support for the understanding of the SANS data. The current experimental analysis has highlighted that the morphology of these polymeric films is characterized by hydrated channels in the bulk amorphous phase alternated to stacks of crystalline lamellae, oriented along the stretching direction.
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Houston, Judith Elizabeth
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The high-intensity option of the SANS diffractometer KWS-2 at JCNS – characterization and performance of the new multi-megahertz detection system
Copenhagen
2018
Munksgaard
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A new detection system based on an array of 3He tubes and innovative fast detection electronics has been installed on the high-intensity small-angle neutron scattering (SANS) diffractometer KWS-2 operated by the Jülich Centre for Neutron Science (JCNS) at the Heinz Meier-Leibnitz Zentrum in Garching, Germany. The new detection system is composed of 18 eight-pack modules of 3He tubes that work independently of one another (each unit has its own processor and electronics). To improve the read-out characteristics and reduce the noise, the detection electronics are mounted in a closed case on the rear of the 3He tubes' frame. The tubes' efficiency is about 85% (for λ = 5 Å) and the resolution slightly better than 8 mm. The new detection system is characterized by a dead-time constant of 3.3 µs per tube and an overall count rate as high as 6 MHz at 10% dead-time loss. Compared with the old detector this is an improvement by a factor of 60. The much higher count rate will shorten the measurement times and thus increase the number of experiments possible in a given time period by the optimal use of the high flux of up to 2 × 108 n cm−2 s−1 at the sample position. Combined with the event-mode operation capability, this will enable new scientific opportunities in the field of structural investigations of small soft-matter and biological systems. The implementation of the detector in the high-intensity concept on KWS-2, its characterization and its performance based on test experiments are reported in this paper.
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2018
0021-8898
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Pipich, Vitaliy
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Densification of Supercritical Carbon Dioxide Accompanied by Droplet Formation When Passing the Widom Line
College Park, Md.
2018
APS
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Thermal density fluctuations of supercritical CO2 were explored using small-angle neutron scattering (SANS), whose amplitude (susceptibility) and correlation length show the expected maximum at the Widom line. At low pressure, the susceptibility is in excellent agreement with the evaluated values on the basis of mass density measurements. At about 20 bar beyond the Widom line, SANS shows the formation of droplets accompanied by an enhanced number density of the supercritical fluid. The corresponding borderline is interpreted as a Frenkel line separating gas- and liquidlike regimes.
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0021-9797
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FZJ-2018-02694
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540
Gvaramia, Manuchar
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Capillary condensation and gelling of microemulsions with clay additives
Amsterdam [u.a.]
2018
Elsevier
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The capillary condensation in bicontinuous microemulsions takes place when two parallel surfaces are narrowed that result in a completely lamellar microemulsion. We expected that this phase transition is also observable when the amount of hydrophilic surfaces from clay particles is raised, because hydrophilic surfaces induce lamellar ordering locally. Using small angle neutron scattering, the structure of micreoemulsions was observed as a function of clay content. The critical concentration is indicated by discontinuous structural changes and depends on the platelet diameter and is explained by the free energy of the platelets competing with the fluctuating medium. The gel phase transition is observed in the spectroscopic measurements where the diffusion motion is widely suppressed in the gel phase, but otherwise superimposes with the membrane undulations.
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Holderer, Olaf
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Frielinghaus, Henrich
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10.1016/j.jcis.2018.04.032
Vol. 525, p. 161 - 165
PERI:(DE-600)1469021-4
161 - 165
Journal of colloid and interface science
525
2018
0021-9797
c.frick@fz-juelich.de
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Strategies for removing multiple scattering effects revisited
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The multiple scattering problem of small angle neutron scattering (SANS) is revisited using differential equations from which different contributions are derived. The coherent scattering is connected to multiple scattering events and the ideal single scattering cross sections can be related to the apparent scattering cross section. The multiple scattering problem of the incoherent scattering is more demanding because the sample geometry – I assumed a slab – matters. I tried to solve this problem analytically, and used Monte Carlo simulations. From all concepts I derived a strategy for a computer program that is capable to remove multiple scattering effects. As a side aspect, I could also remove resolution effects.
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MARIA (magnetism reflectometer with high incident angle) is a world class vertical sample reflectometer dedicated to the investigation of thin films in the fields of magnetism, soft matter and biology. The elliptical vertically focusing guide allows one to measure small samples with a typical size of 1 × 1 cm very efficiently. The double-bounce polarizer and the in situ pumped 3He SEOP (spin-exchange optical pumping) neutron spin filter cell for analysing the polarization of the reflected neutron beam can be moved into the beam in seconds. The polarized flux of MARIA amounts to 5 × 107 n (s cm2)−1 at the sample position with a horizontally collimated beam of 3 mrad, a wavelength of λ = 4.5 Å and a wavelength resolution of Δλ/λ = 10%. In the non-polarized mode a flux of 1.2 × 108 n (s cm2)−1 is achieved in this configuration. MARIA is also capable of grazing-incidence small-angle neutron scattering measurements, using a pinhole collimation with two four-segment slits and an absorber that prevents the focusing of the elliptical guide in the vertical direction.
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0021-9797
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2128/19757
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Lipfert, Frederik
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Stability of near-surface ordering of bicontinuous microemulsions in external shear-fields
Amsterdam [u.a.]
2019
Elsevier
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The lubrication effect of bicontinuous microemulsions describes a facilitated flow along hydrophilic planar surfaces because the fluid forms lamellar domains that can slide off along each other much better than randomly ordered domains. The applicability of this effect is based on the prerequisite of the lamellar structure not being destroyed by external shear-fields. In this paper, we demonstrate that the lamellar structure is highly stable for shear rates of up to 600 s−1 using neutron reflectivity and grazing incidence small angle neutron scattering experiments. The transition structure that consists of perforated lamellae is attacked by the flow, and the bicontinuous microemulsion comes closer to the solid interface when shear is applied. All of this verifies the stability of the lubrication effect for technical applications.
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2019
0021-9797
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He, Xin
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Fluorine-free water-in-ionomer electrolytes for sustainable lithium-ion batteries
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Nature Publishing Group UK
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The continuously increasing number and size of lithium-based batteries developed for large-scale applications raise serious environmental concerns. Herein, we address the issues related to electrolyte toxicity and safety by proposing a “water-in-ionomer” type of electrolyte which replaces organic solvents by water and expensive and toxic fluorinated lithium salts by a non-fluorinated, inexpensive and non-toxic superabsorbing ionomer, lithium polyacrylate. Interestingly, the electrochemical stability window of this electrolyte is extended greatly, even for high water contents. Particularly, the gel with 50 wt% ionomer exhibits an electrochemical stability window of 2.6 V vs. platinum and a conductivity of 6.5 mS cm−1 at 20 °C. Structural investigations suggest that the electrolytes locally self-organize and most likely switch local structures with the change of water content, leading to a 50% gel with good conductivity and elastic properties. A LiTi2(PO4)3/LiMn2O4 lithium-ion cell incorporating this electrolyte provided an average discharge voltage > 1.5 V and a specific energy of 77 Wh kg−1, while for an alternative cell chemistry, i.e., TiO2/LiMn2O4, a further enhanced average output voltage of 2.1 V and an initial specific energy of 124.2 Wh kg−1 are achieved.
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fzj
10.1038/s41467-018-07331-6
Vol. 9, no. 1, p. 5320
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5320
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9
2018
2041-1723
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Control of the stripe domain pattern in L1$_0$ -ordered FePd thin films
Amsterdam
2019
North-Holland Publ. Co.
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L10-ordered FePd thin films with strong perpendicular magnetic anisotropy and self-organized domain patterns have been prepared using molecular beam epitaxy. We demonstrate reproducible growth methods for controlling the strength of the anisotropy and the lateral domain patterns. Neutron scattering experiments have been used to probe the FePd domain structure and were compared with simulations in the framework of the Distorted Wave Born Approximation
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Using neutron methods SANS and PGAA to study evolution of structure and composition of Alkali-doped Polybenzimidazole membranes
New York, NY [u.a.]
2019
Elsevier
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Potassium hydroxide (KOH) doped polybenzimidazole (PBI) membranes are investigated as compelling candidates for water electrolysis applications, drastically reducing the ohmic losses in contrast to thick ZrO2 based diaphragms. Using small angle neutron scattering (SANS) we have found that the structure of the (KOH doped) PBI changes with doping time on a minute time scale, and that the development of the structure is highly dependent on the KOH concentration. This data is correlated with macroscopic measurements of membrane swelling resulting from the doping process which also occurs on a minute time scale. Then, using prompt gamma activation analysis (PGAA) to follow the changes in time of the chemical composition, we have found that the K concentration of these samples only increases slightly with doping times after a very rapid initial uptake, reaching a saturation value that is relatively independent of KOH concentration for long doping times of up to 24 h. However measurements of similarly doped samples show increases in ion-conductivity of nearly 3 fold, and resistivity reductions of over 2 fold on the same time scales. These measurements prove that PGAA is a sensitive method to follow changes in the chemical compositions during doping, while SANS can give information on the sub-micro structural changes of polymer electrolyte membranes. Since these methods can be correlated with ex-situ measurements of composition, resistance, ion-conductivity and macro-structure, the combined use of PGAA and SANS provides a promising means for in-operando study in order to elucidate changes in membrane performance due to electrochemical cycling, as well as to help characterize and optimize doping parameters though in-situ doping measurements, by enabling real-time study of such membrane systems.
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Frielinghaus, Henrich
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The locally columnar model for clay/polymer systems: Connections to scattering experiments
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2019
Elsevier
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A tight connection of scattering to thermodynamic models is missing for clay systems. A new approach called “locally columnar model” gives an attempt for making this connection. The scattering model assumes an up-lining of clay particles with strong paracrystalline order and refers to a chemical potential/distance dependence. The thermodynamic model assumes a bidisperse distance distribution and gives input to the scattering model. Experimentally, polymer/clay systems with many molecular polymer masses were studied showing all very similar scattering curves. While the dominating bulk phase shows only the same weak tendency to stack formation for all molecular polymer masses, one coexisting phase with stronger stack formation was identified. The latter sample was used to determine the thickness of the clay platelets with adsorbed polymer that was then used to model the dominating bulk phase. The comparisons to the theory revealed that (a) most polymers are tightly bound to the clay, and (b) an agreement between the modeling and the theory was achieved. The main result of the experiments is the fraction of free polymers of 1:2400 that are not tightly bound to the clay particles.
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540
Koutsioumpas, Alexandros
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Model-independent recovery of interfacial structure from multi-contrast neutron reflectivity data
[S.l.]
2019
Wiley-Blackwell
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Neutron specular reflectivity at soft interfaces provides sub-nanometre information concerning the molecular distribution of thin films, while the application of contrast variation can highlight the scattering from different parts of the system and lead to an overall reduction in fitting ambiguity. Traditional modelling approaches involve the construction of a trial scattering length density profile based on initial speculation and the subsequent refinement of its parameters through minimization of the discrepancy between the calculated and measured reflectivity. In practice this might produce an artificial bias towards specific sets of solutions. On the other hand, direct inversion of reflectivity data, despite its ability to provide a unique solution, is subject to limitations and experimental complications. Presented here is an integrated indirect Fourier transform/simulated annealing method that, when applied to multiple solvent contrast reflectivity data and within the limits of finite spatial resolution, leads to reliable reconstructions of the interfacial structure without the need for any a priori assumptions. The generality of the method permits its straightforward application in common experimental contrast-variation investigations at the solid/liquid and air/liquid interface.
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2019
1600-5767
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Jaksch, Sebastian
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Long-Range Excitations in Phospholipid Membranes
Amsterdam [u.a.]
2019
Elsevier Science
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We investigated the existence of long-range excitations and correlated structures in phospholipid membranes by means of grazing-incidence neutron spin echo spectroscopy, grazing-incidence small-angle neutron scattering, and corresponding theoretical calculations inspired by smectic-membrane theory. All these methods confirmed the existence of thermal excitations in the plane of the surface of the phospholipid membranes or the corresponding structures, respectively. Also, these measurements revealed a temperature dependence of these excitations. These excitations are associated with 100 nm in-plane correlations around physiological temperatures and of 75 nm at 16∘C. A single excitation has an energy around the μeV-regime. A temperature series revealed a high abundance at physiological temperatures and pronounced long-range in-plane structures, which are strongly suppressed at temperatures below 20∘C. From the length-scales and energy transfers involved we surmise that these excitations may play a role in several functions of the cell membranes such as stability and energy dissipation along the membrane. From a fundamental point of view, the observed behavior of those excitations is congruent with that of a quasi-particle (surface mode phonon, smomon) that exists in the plane of phospholipid membranes.
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Chemistry and physics of lipids
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2019
0009-3084
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Magnetocaloric Mn5Si3 and MnFe4Si3 at variable pressure and temperature
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2019
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The influence of hydrostatic high pressure on the crystal structures and magnetic properties of magnetocaloric Mn5Si3 and MnFe4Si3 was studied with temperature dependent synchrotron powder diffraction, neutron single-crystal diffraction and magnetization measurements. Mn5Si3 shows no indication for any pressure-induced structural phase transition up to 24.2 GPa at room temperature. MnFe4Si3 exhibits no clear indication for any phase transition at high temperatures (296 K–373 K) and high pressures. Anomalies in the lattice parameter at low temperatures indicate a structural response to magnetic ordering. The gradient of decreasing magnetic transition temperature with increasing pressure is dT C/dP ≈ −15 K GPa−1. The transition temperature in MnFe4Si3 can be tuned by pressure in the temperature range relevant for applications, while pressure has hardly any detrimental influence on other key features relevant to magnetocaloric applications (the width of hysteresis, saturation magnetization, magnetocrystalline anisotropy).
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Localised contacts lead to nanosecond hinge motions in dimeric bovine serum albumin
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Domain motions in proteins are crucial for biological function. In the present manuscript, we present a neutron spin-echo spectroscopy (NSE) study of native bovine serum albumin (BSA) in solution. NSE allows to probe both global and internal dynamics of the BSA monomer and dimer equilibrium that is formed in solution. Using a model independent approach, we were able to identify an internal dynamic process in BSA that is visible in addition to global rigid-body diffusion of the BSA monomer and dimer mixture. The observed internal protein motion is characterised by a relaxation time of 43 ns. The overdamped Brownian oscillator was considered as an alternative analytical theory that was able to describe the internal process as first-order approximation. More detailed information on the physical nature of the internal protein motion was extracted from the q-dependent internal diffusion coefficients ΔDeff(q) that were detected by NSE in addition to global rigid-body translational and rotational diffusion. The ΔDeff(q) were interpreted using normal mode analysis based on the available crystal structures of the BSA monomer and dimer as structural test models. Normal mode analysis demonstrates that the observed internal dynamic process can be attributed to bending motion of the BSA dimer. The native BSA monomer does not show any internal dynamics on the time- and length-scales probed by NSE. An intermolecular disulphide bridge or a direct structural contact between the BSA monomers forms a localised link acting as a molecular hinge in the BSA dimer. The effect of that hinge on the observed motion of BSA in the used dimeric structural model is discussed in terms of normal modes in a molecular picture.
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The Multilevel Structure of Sulfonated Syndiotactic-Polystyrene Model Polyelectrolyte Membranes Resolved by Extended Q-Range Contrast Variation SANS
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2019
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Membranes based on sulfonated synditoactic polystyrene (s-sPS) were thoroughly characterized by contrast variation small-angle neutron scattering (SANS) over a wide Q-range in dry and hydrated states. Following special sulfonation and treatment procedures, s-sPS is an attractive material for fuel cells and energy storage applications. The film samples were prepared by solid-state sulfonation, resulting in uniform sulfonation of only the amorphous phase while preserving the crystallinity of the membrane. Fullerenes, which improve the resistance to oxidation decomposition, were incorporated in the membranes. The fullerenes seem to be chiefly located in the amorphous regions of the samples, and do not influence the formation and evolution of the morphologies in the polymer films, as no significant differences were observed in the SANS patterns compared to the fullerenes-free s-sPS membranes, which were investigated in a previous study. The use of uniaxially deformed film samples, and neutron contrast variation allowed for the identification and characterization of different structural levels with sizes between nm and μm, which form and evolve in both the dry and hydrated states. The scattering length density of the crystalline regions was varied using the guest exchange procedure between different toluene isotopologues incorporated into the sPS lattice, while the variation of the scattering properties of the hydrated amorphous regions was achieved using different H2O/D2O mixtures. Due to the deformation of the films, the scattering characteristics of different structures can be distinguished on specific detection sectors and at different detection distances after the sample, depending on their size and orientation.
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2019
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Gvaramia, Manuchar
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Tunable viscosity modification with diluted particles: when particles decrease the viscosity of complex fluids
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2019
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While spherical particles are the most studied viscosity modifiers, they are well known only to increase viscosities, in particular at low concentrations of approx. 1%. Extended studies and theories on non-spherical particles in simple fluids find a more complicated behavior, but still a steady increase with increasing concentration. Involving platelets in combination with complex fluids – in our case a bicontinuous microemulsion – displays an even more complex scenario that we analyze experimentally and theoretically as a function of platelet diameter using small angle neutron scattering, rheology and the theory of the lubrication effect, to find the underlying concepts. The clay particles effectively form membranes in the medium that itself may have lamellar aligned domains and surfactant films in the case of the microemulsion. The two-stage structure of clay and surfactant membranes explains the findings using the theory of the lubrication effect. This confirms that layered domain structures serve for lowest viscosities. Starting from these findings and transferring the condition for low viscosities to other complex fluids, namely crude oils, even lowered viscosities with respect to the pure crude oil were observed. This strengthens our belief that also here layered domains are formed as well. This apparent contradiction of a viscosity reduction by solid particles could lead to a wider range of applications where low viscosities are desired. The same concepts of two-stage layered structures also explain the observed conditions for extremely enhanced viscosities at particle concentrations of 1% that may be interesting for the food industry.
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Appel, Marina
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Proton diffusion in the catalytic layer for high temperature polymer electrolyte fuel cells
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2019
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The present study focuses on quasielastic neutron scattering (QENS) of the proton dynamics in phosphoric acid (PA) inside the catalytic layer of high-temperature polymer electrolyte fuel cells (HT-PEFCs). The nanosecond proton dynamics is investigated on the local length scale around operating temperatures (300 K–430 K) using neutron backscattering spectroscopy. We have investigated the catalyst doped with different amounts of PA in order to understand the distribution of PA inside the layer. Three approaches are considered for the description of proton dynamics: the random jump diffusion model, distribution of diffusion constants and, finally, the trap model. Due to adsorption of the PA on the Pt particles the diffusion of protons in the catalytic layer is different in comparison to the bulk acid. The proton dynamics in the catalytic layer can be described by the random jump diffusion with traps. This diffusion is significantly slower than the diffusion of free PA; this also results in a lower conductivity, which is estimated from the obtained diffusion constant.
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Balacescu, Livia
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Transition between protein-like and polymer-like dynamic behavior: Internal friction in unfolded apomyoglobin depends on denaturing conditions
[London]
2020
Macmillan Publishers Limited, part of Springer Nature
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Equilibrium dynamics of different folding intermediates and denatured states is strongly connected to the exploration of the conformational space on the nanosecond time scale and might have implications in understanding protein folding. For the first time, the same protein system apomyoglobin has been investigated using neutron spin-echo spectroscopy in different states: native-like, partially folded (molten globule) and completely unfolded, following two different unfolding paths: using acid or guanidinium chloride (GdmCl). While the internal dynamics of the native-like state can be understood using normal mode analysis based on high resolution structural information of myoglobin, for the unfolded and even for the molten globule states, models from polymer science are employed. The Zimm model accurately describes the slowly-relaxing, expanded GdmCl-denaturated state, ignoring the individuality of the different aminoacid side chain. The dynamics of the acid unfolded and molten globule state are similar in the framework of the Zimm model with internal friction, where the chains still interact and hinder each other: the first Zimm relaxation time is as large as the internal friction time. Transient formation of secondary structure elements in the acid unfolded and presence of α-helices in the molten globule state lead to internal friction to a similar extent.
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Fuel Cell Electrode Characterization Using Neutron Scattering
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2020
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Electrochemical energy conversion and storage is key for the use of regenerative energies at large scale. A thorough understanding of the individual components, such as the ion conducting membrane and the electrode layers, can be obtained with scattering techniques on atomic to molecular length scales. The largely heterogeneous electrode layers of High-Temperature Polymer Electrolyte Fuel Cells are studied in this work with small- and wide-angle neutron scattering at the same time with the iMATERIA diffractometer at the spallation neutron source at J-PARC, opening a view on structural properties on atomic to mesoscopic length scales. Recent results on the proton mobility from the same samples measured with backscattering spectroscopy are put into relation with the structural findings.
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Morphology of Thin Film Composite Membranes Explored by Small-Angle Neutron Scattering and Positron-Annihilation Lifetime Spectroscopy
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2020
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The morphology of thin film composite (TFC) membranes used in reverse osmosis (RO) and nanofiltration (NF) water treatment was explored with small-angle neutron scattering (SANS) and positron-annihilation lifetime spectroscopy (PALS). The combination of both methods allowed the characterization of the bulk porous structure from a few Å to µm in radius. PALS shows pores of 4.5 Å average radius in a surface layer of about 4 m thickness, which become 40% smaller at the free surface of the membranes. This observation may correlate with the glass state of the involved polymer. Pores of similar size appear in SANS as closely packed pores of 6 Å radius distributed with an average distance of 30 Å. The main effort of SANS was the characterization of the morphology of the porous polysulfone support layer as well as the fibers of the nonwoven fabric layer. Contrast variation using the media H2O/D2O and supercritical CO2 and CD4 identified the polymers of the support layers as well as internal heterogeneities.
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Membranes
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A new neutron depth profiling (NDP) spectrometer has been designed and built for the use at a high intensity focused cold neutron beam of the reflectometer MARIA at the Heinz Maier-Leibnitz Zentrum (MLZ, Germany). The extremely high neutron flux at the sample position of MARIA joined with the multiple charged particle detectors allows less than 10 s sampling rate and paves the way to study the kinetics of Li ions in thin-film microbatteries. The performance of the spectrometer with standard calibration samples and LiNbO3 amorphous thin films is presented; possibilities to operando study the Li distribution inside thin-film rechargeable lithium batteries are discussed.
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Lipid-based nanoparticles, also called vesicles or liposomes, can be used as carriers for drugs or many types of biological macromolecules, including DNA and proteins. Efficiency and speed of cargo delivery are especially high for carrier vesicles that fuse with the cellular plasma membrane. This occurs for lipid mixture containing equal amounts of the cationic lipid DOTAP and a neutral lipid with an additional few percents of an aromatic substance. The fusion ability of such particles depends on lipid composition with phosphoethanolamine (PE) lipids favoring fusion and phosphatidyl-choline (PC) lipids endocytosis. Here, we examined the effects of temperature, ionic strength, osmolality, and pH on fusion efficiency of cationic liposomes with Chinese hamster ovary (CHO) cells. The phase state of liposomes was analyzed by small angle neutron scattering (SANS). Our results showed that PC containing lipid membranes were organized in the lamellar phase. Here, fusion efficiency depended on buffer conditions and remained vanishingly small at physiological conditions. In contrast, SANS indicated the coexistence of very small (~50 nm) objects with larger, most likely lamellar structures for PE containing lipid particles. The fusion of such particles to cell membranes occurred with very high efficiency at all buffer conditions. We hypothesize that the altered phase state resulted in a highly reduced energetic barrier against fusion
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This paper reports on the formation of large area, self assembled, highly ordered monolayers of stearyl alcohol grafted silica nanospheres of ≈50 nm diameter on a silicon substrate based on the drop-casting method. Our novel approach to achieve improved order uses stearyl alcohol as an assistant by adding it to the colloidal NanoParticle (NP) dispersion from which the monolayers are formed. Additionally, a heat treatment step is added, to melt the stearyl alcohol in the monolayer and thereby give the particles more time to further self-assemble, leading to additional improvement in the monolayer quality. The formation of the monolayers is significantly affected by the concentration of the NPs and the stearyl alcohol, the volume of the drop as well as the time of the heat treatment. A high surface coverage and uniform monolayer film of SiO2 NPs is achieved by appropriate control of the above-mentioned preparation parameters. Structural characterization of the obtained SiO2 NP monolayer was done locally by Scanning Electron Microscopy (SEM), and globally by X-ray reflectivity (XRR) and grazing incidence small-angle X-ray scattering (GISAXS), where the data was reproduced by simulation within the Distorted Wave Born Approximation (DWBA). In conclusion, our modified drop-casting method is a simple, inexpensive method, which provides highly ordered self-assembled monolayers of silica particles, if combined with a compatible additive and a heat treatment step. This method might be more general and also applicable to different particles after finding an appropriate additive.
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Pasini, S.
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Fluctuation suppression in microgels by polymer electrolytes
Melville, NY
2020
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Structural details of thermoresponsive, cationically poly(N-iso-propylacrylamide-co-methacrylamido propyl trimethyl ammonium chloride) microgels and the influence of the anionic electrolyte polystyrene sulfonate (PSS) on the internal structure and dynamics of the cationic microgels have been studied with a combination of small angle neutron scattering (SANS) and neutron spin echo (NSE) spectroscopy. While SANS can yield information on the overall size of the particles and on the typical correlation length inside the particles, studying the segmental polymer dynamics with NSE gives access to more internal details, which only appear due to their effect on the polymer motion. The segmental dynamics of the microgels studied in this paper is to a large extent suppressed by the PSS additive. Possible scenarios of the influence of the polyanions on the microgel structure and dynamics are discussed.
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Strain and Electric Field Control of Magnetism in La(1-x)SrxMnO3 Thin Films on Ferroelectric BaTiO3 Substrates
[
2020
IOP73379
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We report on the observation of strain- and magneto-electric coupling in a system consisting of a thin film of ferromagnetic La(1−x)Sr x MnO3 (LSMO, x = 0.5 and 0.3) on a ferroelectric BaTiO3 (BTO) substrate. Pronounced magnetization steps occur at the BTO structural phase transitions. We associate these steps with a strain induced change of the magnetic anisotropy. Temperature dependent magneto-electric coupling could be evidenced by the magnetic response to an applied AC electric field in all ferroelectric phases of the BTO substrate. In a DC electric field, the magnetization changes are asymmetric with respect to the polarity. Polarized neutron reflectometry hints to oxygen migration as possible mechanism for this asymmetry. It also reveals strain-induced magnetization changes throughout most of the thickness of 252 Å (x = 0.5) and 360 Å (x = 0.3), respectively, of the LSMO layer. We conclude that the change of the magnetization depth profile at the interface as previously proposed by ab initio calculations is not the relevant mechanism. Instead strain, oxygen vacancies and frustration at interfacial steps dominate the magnetic response to an applied electric field
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Schiavone, Maria-Maddalena
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The Effects of Temperature and Humidity on the Microstructure of Sulfonated Syndiotactic–polystyrene Ionic Membranes
Basel
2020
MDPI
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Polymeric membranes based on the semi-crystalline syndiotactic–polystyrene (sPS) become hydrophilic, and therefore conductive, following the functionalization of the amorphous phase by the solid-state sulfonation procedure. Because the crystallinity of the material, and thus the mechanical strength of the membranes, is maintained and the resistance to oxidation decomposition can be improved by doping the membranes with fullerenes, the sPS becomes attractive for proton-exchange membranes fuel cells (PEMFC) and energy storage applications. In the current work we report the micro-structural characterization by small-angle neutron scattering (SANS) method of sulfonated sPS films and sPS–fullerene composite membranes at different temperatures between 20 °C and 80 °C, under the relative humidity (RH) level from 10% to 70%. Complementary characterization of membranes was carried out by FTIR, UV-Vis spectroscopy and prompt–γ neutron activation analysis in terms of composition, following the specific preparation and functionalization procedure, and by XRD with respect to crystallinity. The hydrated ionic clusters are formed in the hydrated membrane and shrink slightly with the increasing temperature, which leads to a slight desorption of water at high temperatures. However, it seems that the conductive properties of the membranes do not deteriorate with the increasing temperature and that all membranes equilibrated in liquid water show an increased conductivity at 80 °C compared to the room temperature. The presence of fullerenes in the composite membrane induces a tremendous increase in the conductivity at high temperatures compared to fullerenes-free membranes. Apparently, the observed effects may be related to the formation of additional hydrated pathways in the composite membrane in conjunction with changes in the dynamics of water and polymer.
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2020
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Myelin basic protein (MBP) and its interaction with lipids of the myelin sheath plays an important part in the pathology of multiple sclerosis (MS). Previous studies observed that changes in the myelin lipid composition lead to instabilities and enhanced local curvature of MBP-lipid multilayer structures. We investigated the molecular origin of the instability and found that the diseased lipid membrane has a 25% lower bending rigidity, thus destabilizing smooth >1µm curvature radius structures such as in giant unilamellar vesicles. MBP-mediated assembling of lipid bilayers proceeds in two steps, with a slow second step occurring over many days where native lipid membranes assemble into well-defined multilayer structures, whereas diseased lipid membranes form folded assemblies with high local curvature. For both native and diseased lipid mixtures we find that MBP forms dense liquid phases on top of the lipid membranes mediating attractive membrane interactions. Furthermore, we observe MBP to insert into its bilayer leaflet side in case of the diseased lipid mixture, whereas there is no insertion for the native mixture. Insertion increases the local membrane curvature, and could be caused by a decrease of the sphingomyelin content of the diseased lipid mixture. These findings can help to open a pathway to remyelination strategies.
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Holderer, O.
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Raspberry structures in microgel-silica nanoparticle composite systems
Amsterdam [u.a.]
2021
Elsevier
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Composite materials consisting of responsive microgels together with additional nanoparticles might provide new and “smart” functionality, e.g. uptake and release of nanoparticles, or special mechanical or rheological properties of a solution. Here, composites consisting of PNIPAM microgels and silica nanoparticles have been investigated by CryoTEM and neutron scattering techniques. The formation of “raspberry” like core–shell structures with a silica nanoparticle layer around the microgel core has been observed.
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Kruteva, M.
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Self-Similar Dynamics of Large Polymer Rings: A Neutron Spin Echo Study
College Park, Md.
2020
APS
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This work clarifies the self-similar dynamics of large polymer rings using pulsed-field gradient nuclear magnetic resonance and neutron spin echo spectroscopy. We find center of mass diffusion taking place in three dynamic regimes starting (i) with a strongly subdiffusive domain ⟨r2(t)⟩com∼tα (0.4≤α≤0.65); (ii) a second subdiffusive region ⟨r2(t)⟩com∼t0.75 that (iii) finally crosses over to Fickian diffusion. While the t0.75 range previously has been found in simulations and was predicted by theory, we attribute the first to the effect of cooperative dynamics resulting from the correlation hole potential. The internal dynamics at scales below the elementary loop size is well described by ring Rouse motion. At larger scales the dynamics is self-similar and follows very well the predictions of the scaling models with preference for the self-consistent fractal loopy globule model.
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Polymorphic phase transition in liquid and supercritical carbon dioxide
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We present experiments on molecular density fluctuations in liquid and supercritical (SC) CO2 using small-angle neutron scattering. Thermal density fluctuations in SC-CO2 determine susceptibility and correlation length identifying the Widom line at their maxima. Droplet formation occurs at the gas–liquid line and between 20 and 60 bar above the Widom line, the corresponding borderline identified as the Frenkel line. The droplets start to form spheres of constant radius of ≈ 45 Å and transform into rods and globules at higher pressure. Droplet formation represents a liquid–liquid (polymorphic) phase transition of the same composition but different density, whose difference defines its order parameter. Polymorphism in CO2 is a new observation stimulating interesting discussions on the topics of gas-like to liquid-like transition in SC fluids and polymorphism since CO2 represents a “simple” van der Waals liquid in contrast to water, which is the most widely studied liquid showing polymorphism in its supercooled state.
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Tuning the Co/Sr stoichiometry of SrCoO$_{2.5}$ thin films by RHEED assisted MBEgrowth
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2020
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Strontium cobaltite (SrCoO2.5+δ, SCO) is a fascinating material because of its topotactic structural phase transition caused by a change in oxygen stoichiometry. In the brownmillerite phase (δ = 0) it is an insulating antiferromagnet whereas in the perovskite phase (δ = 0.5) it is a conducting ferromagnet. In contrast, the impact of the varying Co/Sr stoichiometry on the structure has not yet been studied in SCO thin films. Using molecular beam epitaxy we have fabricated SCO thin films of varying Co/Sr stoichiometry. Films with Co excess exhibit a brownmillerite crystal structure with CoO precipitates within the thin film and on the surface. Co deficient films are amorphous. Only for 1:1 stoichiometry a pure brownmillerite structure is present. We find a clear dependence of the Reflection High Energy Electron Diffraction (RHEED) pattern of these thin films on the stoichiometry. Interestingly, RHEED is very sensitive to a Co excess of less than 12% while x-ray diffraction fails to reveal that difference. Hence, using RHEED, the stoichiometry of SCO can be evaluated and tuned in-situ to a high degree of precision, which allows for a quick adjustment of the growth parameters during a sample series.
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Performance of a Position Sensitive Neutron Scintillation Detector based on Silicon Photomultipliers
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2020
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In recent years, the price increase of 3He has triggered the search for alternative neutron detectors. One of the viable options is a scintillation based neutron detector. Usually, Photomultiplier tubes (PMTs) are used in these detectors for photodetection. However, the increase in performance requirements such as the operability in magnetic field and spatial resolution, necessitates an advanced neutron detector. Therefore, we developed a detector prototype with an active area of 13 cm x 13 cm using Silicon photomultipliers (SiPM). As compared to PMTs, SiPMs offer more compactness, more robustness and a lower sensitivity to magnetic fields. The final detector is aimed to be used in the future at the TREFF instrument of the Heinz Maier-Leibnitz Zentrum (MLZ) in Garching, Germany for neutron reflectometry (NR). First measurements were carried out at TREFF and at the dedicated detector test instrument V17 at BER-II of HZB in Berlin, Germany. In this work, we report the results for detection efficiency, gamma discrimination, two-dimensional position resolution, count rate, and detection linearity.
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Grazing incidence small-angle neutron scattering (GISANS) provides access to interfacial properties, e.g., in soft matter on polymers adsorbed at a solid substrate. Simulations in the frame of the distorted wave Born approximation using the BornAgain software allow to understand and quantify the scattering pattern above and below the sample horizon, in reflection and transmission, respectively. The small-angle scattering from the interfacial layer, visible around the transmitted beam, which might contribute also on the side of the reflected beam, can be understood in this way and be included into the analysis. Background reduction by optimized sample cell design is supported by simulations, paving the way for an optimized GISANS cell.
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Revealing the Absolute Direction of the Dzyaloshinskii-Moriya Interaction in Prototypical Weak Ferromagnets by Polarized Neutrons
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2021
APS
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Polarized neutron diffraction (PND) is a powerful technique to distinguish a weak magnetic contribution from the total scattering intensity. It can provide a detailed insight into the microscopic spin ordering at the unit cell level, but also into the mesoscopic magnetic ordering, like different types of domain populations. Here we report on the application of this technique to the long-standing problem of determining the absolute direction of the Dzyaloshinskii-Moriya vector in relation to the crystal structure. The proposed PND method, based on the measurement of one representative reflection, is easy to perform and straightforward to interpret. The absolute sign of the Dzyaloshinskii-Moriya interaction (DMI) in MnCO3 has been independently determined by PND and found to be in agreement with recent results obtained by resonant magnetic synchrotron scattering. This validates the method. In addition, the absolute DMI vector direction in the prototypical room-temperature weak ferromagnet α-Fe2O3 (hematite) has been determined for the first time. To demonstrate the generality of our method, further examples with different symmetries are also presented. Ab initio calculations of the resulting weak noncollinear magnetization using the quantum espresso package, considering DMI in addition to the symmetric magnetic exchange interaction, were also conducted and found to be in agreement with the experimental results from PND.
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Van Herck, Walter
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Deep learning for X-ray or neutron scattering under grazing-incidence: extraction of distributions
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2021
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Grazing-incidence small-angle scattering (GISAS) is a technique of significant importance for the investigation of thin multilayered films containing nano-sized objects. It provides morphology information averaged over the sample area. However, this averaging together with multiple reflections and the well-known phase problem make the data analysis challenging and time consuming. In the present paper we show that densely connected neural networks (DenseNets) can be applied for GISAS data analysis and deliver fast and plausible results. The extraction of the rotational distributions of hexagonal nanoparticle arrangements is taken as a case study.
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0031-9007
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Zamponi, M.
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Cooperative Chain Dynamics of Tracer Chains in Highly Entangled Polyethylene Melts
College Park, Md.
2021
APS
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By neutron spin echo spectroscopy, we have studied the center of mass motion of short tracer chains on the molecular length scale within a highly entangled polymer matrix. The center of mass mean square displacements of the tracers independent of their molecular weight is subdiffusive at short times until it has reached the size of the tube d; then, a crossover to Fickian diffusion takes place. This observation cannot be understood within the tube model of reptation, but is rationalized as a result of important interchain couplings that lead to cooperative chain motion within the entanglement volume ∼d3. Thus, the cooperative tracer chain motions are limited by the tube size d. If the center of mass displacement exceeds this size, uncorrelated Fickian diffusion takes over. Compared to the prediction of the Rouse model we observe a significantly reduced contribution of the tracer’s internal modes to the spectra corroborating the finding of cooperative rather than Rouse dynamics within d3.
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0031-9007
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20221001113512.0
10.3390/membranes11060413
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Pipich, Vitaliy
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Silica Fouling in Reverse Osmosis Systems–Operando Small-Angle Neutron Scattering Studies
Basel
2021
MDPI
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We present operando small-angle neutron scattering (SANS) experiments on silica fouling at two reverse osmose (RO) membranes under almost realistic conditions of practiced RO desalination technique. To its realization, two cells were designed for pressure fields and tangential feed cross-flows up to 50 bar and 36 L/h, one cell equipped with the membrane and the other one as an empty cell to measure the feed solution in parallel far from the membrane. We studied several aqueous silica dispersions combining the parameters of colloidal radius, volume fraction, and ionic strength. A relevant result is the observation of Bragg diffraction as part of the SANS scattering pattern, representing a crystalline cake layer of simple cubic lattice structure. Other relevant parameters are silica colloidal size and volume fraction far from and above the membrane, as well as the lattice parameter of the silica cake layer, its volume fraction, thickness, and porosity in comparison with the corresponding permeate flux. The experiments show that the formation of cake layer depends to a large extent on colloidal size, ionic strength and cross-flow. Cake layer formation proved to be a reversible process, which could be dissolved at larger cross-flow. Only in one case we observed an irreversible cake layer formation showing the characteristics of an unstable phase transition. We likewise observed enhanced silica concentration and/or cake formation above the membrane, giving indication of a first order liquid–solid phase transformation.
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Forschungs-Neutronenquelle Heinz Maier-Leibnitz
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Vol. 11, no. 6, p. 413 -
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413 -
Membranes
11
2021
2077-0375
h.lexis@fz-juelich.de
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Bhatnagar-Schöffmann, Tanvi
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Differentiation between strain and charge mediated magnetoelectric coupling in La 0.7 Sr 0.3 MnO 3 / Pb(Mg 1/3 Nb 2/3 ) 0.7 Ti 0.3 O 3 (001)
[London]
2021
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Magnetoelectric (ME) coupling in La0.7Sr0.3MnO3/Pb(Mg1/3Nb2/3)0.7Ti0.3O3 (LSMO/PMN–PT (001)) has been probed in the past years to identify the underlying mechanism behind it. PMN–PT, which is well known for its excellent piezoelectric properties, also exhibits ferroelectricity. This motivates our interest to differentiate which effect is dominant for this 'voltage control of magnetism'. Here, we present results for the ME coupling at different temperatures: 300 K and 80 K. In this article we discuss and explain, how the nature of ME coupling is influenced by different parameters such as magnetic field, electric field, directional dependence (hard axis, easy axis) and temperature. Owing to large lattice mismatch between LSMO and PMN–PT, the strain-mediated coupling is strongly prevalent, however the change in strain behaviour from butterfly loop to linear loop is observed as a function of temperature. ME measurements are performed along hard axis [100] and easy axis [110] of LSMO in the presence of remanent magnetic field which showcases the pure influence of electric field on the system, resulting in a combination of strain- and charge-mediated coupling. The magnetic depth profile is probed by polarized neutron reflectometry as a function of electric field which demonstrates the existence of an interlayer with reduced nuclear scattering length density and reduced magnetic scattering length density at the interface. From transmission electron microscopy, stoichiometric variations are observed due to the presence of Mn3O4 particles at the interface.
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Nandakumaran, Nileena
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Unravelling Magnetic Nanochain Formation in Dispersion for In Vivo Applications
Weinheim
2021
Wiley-VCH
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Self-assembly of iron oxide nanoparticles (IONPs) into 1D chains is appealing, because of their biocompatibility and higher mobility compared to 2D/3D assemblies while traversing the circulatory passages and blood vessels for in vivo biomedical applications. In this work, parameters such as size, concentration, composition, and magnetic field, responsible for chain formation of IONPs in a dispersion as opposed to spatially confining substrates, are examined. In particular, the monodisperse 27 nm IONPs synthesized by an extended LaMer mechanism are shown to form chains at 4 mT, which are lengthened with applied field reaching 270 nm at 2.2 T. The chain lengths are completely reversible in field. Using a combination of scattering methods and reverse Monte Carlo simulations the formation of chains is directly visualized. The visualization of real-space IONPs assemblies formed in dispersions presents a novel tool for biomedical researchers. This allows for rapid exploration of the behavior of IONPs in solution in a broad parameter space and unambiguous extraction of the parameters of the equilibrium structures. Additionally, it can be extended to study novel assemblies formed by more complex geometries of IONPs.
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10.1002/adma.202008683
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2008683
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33
2021
1521-4095
h.lexis@fz-juelich.de
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Distribution and orientation of nerve fibers and myelin assembly in a brain section retrieved by small-angle neutron scattering
[London]
2021
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The structural connectivity of the brain has been addressed by various imaging techniques such as diffusion weighted magnetic resonance imaging (DWMRI) or specific microscopic approaches based on histological staining or label-free using polarized light (e.g., three-dimensional Polarized Light Imaging (3D-PLI), Optical Coherence Tomography (OCT)). These methods are sensitive to different properties of the fiber enwrapping myelin sheaths i.e. the distribution of myelin basic protein (histology), the apparent diffusion coefficient of water molecules restricted in their movements by the myelin sheath (DWMRI), and the birefringence of the oriented myelin lipid bilayers (3D-PLI, OCT). We show that the orientation and distribution of nerve fibers as well as myelin in thin brain sections can be determined using scanning small angle neutron scattering (sSANS). Neutrons are scattered from the fiber assembly causing anisotropic diffuse small-angle scattering and Bragg peaks related to the highly ordered periodic myelin multilayer structure. The scattering anisotropy, intensity, and angular position of the Bragg peaks can be mapped across the entire brain section. This enables mapping of the fiber and myelin distribution and their orientation in a thin brain section, which was validated by 3D-PLI. The experiments became possible by optimizing the neutron beam collimation to highest flux and enhancing the myelin contrast by deuteration. This method is very sensitive to small microstructures of biological tissue and can directly extract information on the average fiber orientation and even myelin membrane thickness. The present results pave the way toward bio-imaging for detecting structural aberrations causing neurological diseases in future.
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Zhu, Fengfeng
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Topological magnon insulators in two-dimensional van der Waals ferromagnets CrSiTe3 and CrGeTe3 : Toward intrinsic gap-tunability
Washington, DC [u.a.]
2021
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The bosonic analogs of topological insulators have been proposed in numerous theoretical works, but their experimental realization is still very rare, especially for spin systems. Recently, two-dimensional (2D) honeycomb van der Waals ferromagnets have emerged as a new platform for topological spin excitations. Here, via a comprehensive inelastic neutron scattering study and theoretical analysis of the spin-wave excitations, we report the realization of topological magnon insulators in CrXTe3 (X = Si, Ge) compounds. The nontrivial nature and intrinsic tunability of the gap opening at the magnon band-crossing Dirac points are confirmed, while the emergence of the corresponding in-gap topological edge states is demonstrated theoretically. The realization of topological magnon insulators with intrinsic gap-unability in this class of remarkable 2D materials will undoubtedly lead to new and fascinating technological applications in the domain of magnonics and topological spintronics.
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Signature of antiphase boundaries in iron oxide nanoparticles
[S.l.]
2021
Wiley-Blackwell
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Iron oxide nanoparticles find a wide variety of applications, including targeted drug delivery and hyperthermia in advanced cancer treatment methods. An important property of these particles is their maximum net magnetization, which has been repeatedly reported to be drastically lower than the bulk reference value. Previous studies have shown that planar lattice defects known as antiphase boundaries (APBs) have an important influence on the particle magnetization. The influence of APBs on the atomic spin structure of nanoparticles with the γ-Fe2O3 composition is examined via Monte Carlo simulations, explicitly considering dipole–dipole interactions between the magnetic moments that have previously only been approximated. For a single APB passing through the particle centre, a reduction in the magnetization of 3.9% (for 9 nm particles) to 7.9% (for 5 nm particles) is found in saturation fields of 1.5 T compared with a particle without this defect. Additionally, on the basis of Debye scattering equation simulations, the influence of APBs on X-ray powder diffraction patterns is shown. The Fourier transform of the APB peak profile is developed to be used in a whole powder pattern modelling approach to determine the presence of APBs and quantify them by fits to powder diffraction patterns. This is demonstrated on experimental data, where it could be shown that the number of APBs is related to the observed reduction in magnetization.
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Magnetic order and sign of the Dzyaloshinskii-Moriya interaction in 2D antiferromagnet Ba2CoGe2O7 under applied magnetic field
New York, NY
2022
IEEE
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The Dzyaloshinskii-Moriya interaction (DMI), that is the antisymmetric part of the exchange coupling tensor, favors the perpendicular arrangement of magnetic moment, thus, induces canting in otherwise collinear structures. The DMI is the prerequisite for the emergence of weak ferromagnetism in antiferromagnets, but can stabilize twisted magnetic textures, such as spin spirals, soliton lattices and magnetic skyrmions. While the magnitude of the DMI determines the canting angle of adjacent spins, its sign dictates the sense of the spin rotation. Based on a focused polarized neutron diffraction (PND) study, combined with symmetry analysis, we determine the sign of the DMI in the unconventional multiferroic Ba2CoGe2O7 and reveal its detailed magnetic structure in magnetic fields applied in the tetragonal plane. As PND gives unique access to the scattering contribution from the phase-sensitive nuclear-magnetic interference, it is a valuable tool for a straightforward DMI sign determination in bulk materials and allows to disclose even very weak magnetic moments. Remarkably, the sign of the DMI could be determined from the PND measurement of a single reflection which is demonstrated to be reliable for a large range of applied magnetic field directions and values.
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Schiavone, Maria Maddalena
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On the Proton Conduction Pathways in Polyelectrolyte Membranes Based on Syndiotactic-Polystyrene
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10.1080/10448632.2021.1997310
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530
Su, Yixi
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Topology Meets Correlation: Neutron Scattering from Correlated Topological Materials
London [u.a.]
2021
Taylor and Francis
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Teixeira Parente, Mario
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Benchmarking Autonomous Scattering Experiments Illustrated on TAS
2022
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With the advancement of artificial intelligence and machine learning methods, autonomous approaches are recognized to have great potential for performing more efficient scattering experiments. In our view, it is crucial for such approaches to provide thorough evidence about respective performance improvements in order to increase acceptance within a scientific community. Therefore, we propose a benchmarking procedure designed as a cost-benefit analysis that is applicable to any scattering method sequentially collecting data during an experiment. For a given approach, the performance assessment is based on how much benefit, given a certain cost budget, it is able to acquire in predefined test cases. Different approaches thus get a chance for comparison and can make their advantages explicit and visible. Key components of the procedure, i.e., cost measures, benefit measures, and test cases, are made precise for the setting of three-axes spectrometry (TAS) as an illustration. Finally, we discuss neglected aspects and possible extensions for the TAS setting and comment on the procedure’s applicability to other scattering methods. A Python implementation of the procedure to simplify its utilization by interested researchers from the field is also provided.
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Frielinghaus, H.
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Ionic Liquid (EmimAc)-Water Mixture Confined in Nanoporous Glass Matrices Studied With High-Resolution Neutron Spectroscopy
Lausanne
2022
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We report on the structure and diffusion behaviour of the various constituent molecules in ionic liquid (IL) mixtures under confinement in nanoporous glasses. X-Ray diffraction measurements indicate that the ions adopt a lamellar arrangement under confinement. Furthermore, using selective deuteration in combination with high resolution neutron spectroscopy reveals how the dynamics and the activation energy of the IL is affected by different confinement conditions (pore sizes 50 Å and 135 Å) and different temperatures (265 and 318 K). With different deuteration schemes we could separate the different motions of acetate and water. The confinement leads to distortions of the domains, which gives more room for diffusion. In the smaller pores, the stronger distortion gives even more room such that the hydrogen bonds between acetate and water seem to be even stronger than in bulk and weaker confinement. The results are discussed in the context of previous measurements on dry samples.
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Wellert, Stefan
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10.3389/frsfm.2022.887610
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Frontiers in soft matter
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2022
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10.1103/PhysRevX.12.021029
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2128/31197
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Schweika, W.
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Chiral Spin Liquid Ground State in YBaCo 3 FeO 7
College Park, Md.
2022
APS
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A chiral spin liquid state is discovered in the highly frustrated, noncentrosymmetric swedenborgite compound YBaCo3FeO7, a layered kagome system of hexagonal symmetry, by advanced polarized neutron scattering from a single domain crystalline sample. The observed diffuse magnetic neutron scattering has an antisymmetric property that relates to its specific chirality, which consists of three cycloidal waves perpendicular to the c axis, forming an entity of cylindrical symmetry. Chirality and symmetry agree with relevant antisymmetric exchanges arising from broken spatial parity. Applying a Fourier analysis to the chiral interference pattern, with distinction between kagome sites and the connecting trigonal interlayer sites of threefold symmetry, the chiral spin correlation function is determined. Characteristic chiral waves originate from the trigonal sites and extend over several periods in the kagome planes. The chiral spin liquid is remarkably stable at low temperatures despite strong antiferromagnetic spin exchange. The observation raises a challenge, since the commonly accepted ground states in condensed matter either have crystalline long-range order or form a quantum liquid. We show that, within the classical theory of magnetic order, a disordered ground state may arise from chirality. The present scenario, with antisymmetric exchange acting as a frustrating gauge background that stabilizes local spin lumps, is similar to the avoided phase transition in coupled gauge and matter fields for subnuclear particles.
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Recent scattering approaches to structure and dynamics of polymer nanocomposites
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Jaksch, Sebastian
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The GISANS instrument at the HBS
Amsterdam
2023
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This manuscript describes a concept of a grazing incidence small-angle neutron scattering (GISANS) instrument for the high brilliance source (HBS). The HBS being a compact pulsed neutron source using a moderate energy proton accelerator which allows for very compact moderators and shielding, and flexible pulse repetition rates. Similar to many other instrument concepts for this source, the lowest proposed HBS pulse frequency of 24 Hz with a relatively large detector distance is the optimal choice for the instrument described here in terms of obtained intensity and Q-range (i.e. scattering vector range). Such a configuration has the added advantage of good Q-resolution, which is important when scattering depths need to be resolved well. This is especially the case for GISANS when the incident angle is close to the critical angle of total reflection. The performance obtained from detailed ray-tracing computer simulations predict a high performance instrument that will be comparable to reflectometers and small angle neutron scattering (SANS) instruments at high-flux reactor sources such as the Forschungsreaktor Munich (FRM-2) and others.
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10.1016/j.nima.2022.167919
p. 167919 -
PERI:(DE-600)1466532-3
167919
Nuclear instruments & methods in physics research / A
1048
2023
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MLZ User Meeting and German Neutron Scattering Conference 2020: Meetings without Meeting….
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Taylor and Francis
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5 - 5
Neutron news
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2021
1044-8632
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20231001200149.0
10.1021/acsphyschemau.2c00057
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36968449
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FZJ-2023-01307
530
Chua, Yeong Zen
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Determination of Cooperativity Length in a Glass-Forming Polymer
Washington, DC
2023
American Chemical Society
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To describe the properties of glass-forming liquids, the concepts of a cooperativity length or the size of cooperatively rearranging regions are widely employed. Their knowledge is of outstanding importance for the understanding of both thermodynamic and kinetic properties of the systems under consideration and the mechanisms of crystallization processes. By this reason, methods of experimental determination of this quantity are of outstanding importance. Proceeding in this direction, we determine the so-called cooperativity number and, based on it, the cooperativity length by experimental measurements utilizing AC calorimetry and quasi-elastic neutron scattering (QENS) at comparable times. The results obtained are different in dependence on whether temperature fluctuations in the considered nanoscale subsystems are either accounted for or neglected in the theoretical treatment. It is still an open question, which of these mutually exclusive approaches is the correct one. As shown in the present paper on the example of poly(ethyl methacrylate) (PEMA), the cooperative length of about 1 nm at 400 K and a characteristic time of ca. 2 μs determined from QENS coincide most consistently with the cooperativity length determined from AC calorimetry measurements if the effect of temperature fluctuations is incorporated in the description. This conclusion indicates that─accounting for temperature fluctuations─the characteristic length can be derived by thermodynamic considerations from the specific parameters of the liquid at the glass transition and that temperature does fluctuate in small subsystems.
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172–180
ACS physical chemistry Au
3
2023
2694-2445
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http://juser.fz-juelich.de/record/1005108/files/Invoice_APC600374485.pdf
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20231028200156.0
10.1103/PhysRevResearch.5.023053
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2128/34403
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FZJ-2023-01741
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Frielinghaus, Henrich
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Experimental critical dynamics of 3-methyl pyridine/D$_2$O mixtures without and with antagonistic salt
College Park, MD
2023
APS
article
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We observed the criticality in the structure and dynamics of a 3d- and 2d-Ising system consisting of 3-methyl pyridine (3MP) / D2O without and with antagonistic salt. We could describe both dynamic criticalities by the Kawasaki crossover function. The dynamic critical exponent was z=0.063±0.020 and 0.005±0.019 for 3 and 2 dimensions, which confirms earlier observations in the 3d case and confirms expectations in the 2d case. The amplitudes of the critical dynamics are governed by the bare viscosities experimentally, and by the coefficient R theoretically (latter is proportional to (4−d)−1 with the dimensionality d). This finding is in accordance with the lubrication effect that is also connected to lamellar systems of the Brazovskii criticality . This lubrication effect is tightly connected to a laminar flow enforced by the domain structure and also holds for our 2d-Ising system. The experimental techniques employed were small angle neutron and x-rays scattering (SANS and SAXS) for the static criticality and dynamic light scattering (DLS) and neutron spin echo spectroscopy (NSE) for the critical dynamics. Furthermore, the criticality of the viscosities was measured.
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Polymers, Soft Nano Particles and Proteins
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Dubey, Purushottam
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023053
Physical review research
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2023
2643-1564
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Teixeira Parente, Mario
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Active learning-assisted neutron spectroscopy with log-Gaussian processes
2023
Nature Publishing Group
article
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1683870930_12445
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Neutron scattering experiments at three-axes spectrometers (TAS) investigate magnetic and lattice excitations by measuring intensity distributions to understand the origins of materials properties. The high demand and limited availability of beam time for TAS experiments however raise the natural question whether we can improve their efficiency and make better use of the experimenter’s time. In fact, there are a number of scientific problems that require searching for signals, which may be time consuming and inefficient if done manually due to measurements in uninformative regions. Here, we describe a probabilistic active learning approach that not only runs autonomously, i.e., without human interference, but can also directly provide locations for informative measurements in a mathematically sound and methodologically robust way by exploiting log-Gaussian processes. Ultimately, the resulting benefits can be demonstrated on a real TAS experiment and a benchmark including numerous different excitations.
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Condensed Matter Physics
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Instrument and Method Development
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Forschungs-Neutronenquelle Heinz Maier-Leibnitz
PANDA: Cold three axes spectrometer
SR2
EXP:(DE-MLZ)FRMII-20140101
EXP:(DE-MLZ)PANDA-20140101
EXP:(DE-MLZ)PANDA-20140101
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Brandl, Georg
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Franz, Christian
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Stuhr, Uwe
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Ganeva, Marina
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Schneidewind, Astrid
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10.1038/s41467-023-37418-8
Vol. 14, no. 1, p. 2246
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2023
2041-1723
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http://juser.fz-juelich.de/record/1006875/files/s41467-023-37418-8.pdf
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65000
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Stekiel, Michal
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Incommensurate antiferromagnetic order in CePtAl 3
College Park, MD
2023
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We report on a neutron diffraction study of single-crystal CePtAl3 complemented by measurements of the specific heat under applied magnetic field. Below TN ≈ 3 K, CePtAl3 develops incommensurate antiferromagneticorder with a single modulation vector k = (0.676 0 0). Residual magnetic scattering intensity above TN and a broadening of the specific heat anomaly at TN may be consistently described in terms of a Gaussiandistribution of transition temperatures with a standard deviation σ ≈ 0.5 K. The distribution of TN may be attributed to the observation of occupational and positional disorder between the Pt and Al sites consistent withstructural information inferred from neutron diffraction. Measurements under magnetic field reveal changes of the magnetic domain populations when the field is applied along the [0 1 0] direction consistent with a transitionfrom cycloidal to amplitude-modulated magnetic order ∼2.5 T.
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Multiscale Structural Insight into Dairy Products and Plant-Based Alternatives by Scattering and Imaging Techniques
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The metallic compound Mn5Si3 hosts a series of antiferromagnetic phases that can be controlled by external stimuli, such as temperature and magnetic field. In this work, we investigate the spin-excitation spectrum of bulk Mn5Si3 by combining inelastic neutron scattering measurements and density functional theory calculations. We study the evolution of the dynamical response under external parameters and demonstrate that the spin dynamics of each phase is robust against any combination of temperature and magnetic field. In particular, the high-energy spin dynamics is very characteristic of the different phases consisting of either spin waves or broad fluctuation patterns.
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Topological magnons driven by the Dzyaloshinskii-Moriya interaction in the centrosymmetric ferromagnet Mn5Ge3
[London]
2023
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The phase of the quantum-mechanical wave function can encode a topological structure with wide-ranging physical consequences, such as anomalous transport effects and the existence of edge states robust against perturbations. While this has been exhaustively demonstrated for electrons, properties associated with the elementary quasiparticles in magnetic materials are still underexplored. Here, we show theoretically and via inelastic neutron scattering experiments that the bulk ferromagnet Mn5Ge3 hosts gapped topological Dirac magnons. Although inversion symmetry prohibits a net Dzyaloshinskii-Moriya interaction in the unit cell, it is locally allowed and is responsible for the gap opening in the magnon spectrum. This gap is predicted and experimentally verified to close by rotating the magnetization away from the c-axis with an applied magnetic field. Hence, Mn5Ge3 realizes a gapped Dirac magnon material in three dimensions. Its tunability by chemical doping or by thin film nanostructuring defines an exciting new platform to explore and design topological magnons. More generally, our experimental route to verify and control the topological character of the magnons is applicable to bulk centrosymmetric hexagonal materials, which calls for systematic investigation.
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