Measurement of self-diffusion in thin samples using a novel one-sided NMR magnet

Panesar, Kuldeep; Hugon, Cédric; Aubert, G.; Judeinstein, Patrick; Zanotti, Jean-Marc; Sakellariou, Dimitrios

doi:10.1016/j.micromeso.2013.04.016

Cited by 9 publications

(3 citation statements)

References 22 publications

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“…Many single sided NMR systems have been proposed in the literature [13]. Our approach to magnet design is based on the Spherical Harmonic Decomposition methodology to lead to a 12-fold cylindrically symmetric one-sided constant-gradient magnet without pole pieces [14,15], which has been used already to measure onedimensional proton density profiles as well as relaxations and diffusions [16,17]. Our permanent magnet is a cylinder of 24 cm in diameter, 22 cm in height containing NdFeB magnets and weights ∼ 40 kg.…”

Section: A Home-made Portable Single-sided Nmr Setupmentioning

confidence: 99%

Coupling NMR to SANS: Addressing at once structure and dynamics in soft matter

Oliveira‐Silva

Bélime

Cœur

et al. 2020

JNR

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In soft condensed matter, Small Angle Neutron Scattering (SANS) is a central tool to probe structures with characteristic sizes ranging from 1 to 100 nm. However, when used as a standalone technique, the dynamic properties of the sample are not accessible. Nuclear Magnetic Resonance (NMR) is a versatile technique which can easily probe dynamical information. Here, we report on the coupling of a low-field NMR system to a SANS instrument. We show that this original setup makes it possible to obtain structural information and to simultaneously extract in situ on a same sample, long-range translational diffusion coefficient, T 1 and T 2 nuclear spin relaxation times. Such a feature is of major interest when a sample experiences a transient physical state or evolves rapidly. We illustrate the capabilities of alliancing these experimental methods by following the critical temperature-induced phase separation of a concentrated Poly(Methacrylic Acid) solution at its Lower Critical Solution Temperature. The characteristic size related to the domain growth of the polymer-rich phase of the gel is monitored by the evolution of the SANS spectra, while the dynamics of the sol phase (H 2 O and polymer) is simultaneously characterized by NMR by measuring T 1 , T 2 and the diffusion coefficient. Great care has been taken to design a cell able to optimize the thermalization of the sample and in particular its equilibration time. Details are given on the sample cell specifically designed and manufactured for these experiments. The acquisition time needed to reach good signal-to-noise ratios, for both NMR and SANS, match: it is of the order of one hour. Altogether, we show that in situ low-field NMR/SANS coupling the NMR is meaningful and is a promising experimental approach.

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Section: A Home-made Portable Single-sided Nmr Setupmentioning

confidence: 99%

Coupling NMR to SANS: Addressing at once structure and dynamics in soft matter

Oliveira‐Silva

Bélime

Cœur

et al. 2020

JNR

View full text Add to dashboard Cite

show abstract

“…Although these systems are a very active field of research, the actual technical implementation as high-performance supercapacitors remains challenging. One of the reasons is the relatively high viscosity of ionic liquids [8,10,11], resulting in slow ion dynamics [8,12]. While some studies find increased dynamics in the case of carbon nanoconfinement [13][14][15][16], others see a clear slowdown [17][18][19][20].…”

Section: Introductionmentioning

confidence: 99%

Ionic liquid dynamics in nanoporous carbon: A pore-size- and temperature-dependent neutron spectroscopy study on supercapacitor materials

Busch

Hofmann

Frick

et al. 2020

Phys. Rev. Materials

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The influence of spatial confinement on the thermally excited stochastic cation dynamics of the roomtemperature ionic liquid 1-N-butylpyridinium bis-[(trifluoromethyl)sulfonyl]imide ([BuPy][Tf 2 N]) inside porous carbide-derived carbons with various pore sizes in the sub-to a few nanometer range is investigated by quasielastic neutron spectroscopy. Using the potential of fixed window scans, i.e., scanning a sample parameter, while observing solely one specific energy transfer value, an overview of the dynamic landscape within a wide temperature range is obtained. It is shown that already these data provide a quite comprehensive understanding of the confinement-induced alteration of the molecular mobility in comparison to the bulk. A complementary, more detailed analysis of full energy transfer spectra at selected temperatures reveals two translational diffusive processes on different time scales. Both are considerably slower than in the bulk liquid and show a decrease of the respective self-diffusion coefficients with decreasing nanopore size. Different thermal activation energies for molecular self-diffusion in nanoporous carbons with similar pore size indicate the importance of pore morphology on the molecular mobility, beyond the pure degree of confinement. In spite of the dynamic slowing down we can show that the temperature range of the liquid state upon nanoconfinement is remarkably extended to much lower temperatures, which is beneficial for potential technical applications of such systems.

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“…One of the reasons is the relatively high viscosity of ionic liquids [8,10,11], resulting in slow ion dynamics. [8,12] While some studies find increased dynamics in the case of carbon nanoconfinement [13][14][15][16], others see a clear slowdown. [17][18][19][20] Additionally, ionic liquids tend to layer at solid interfaces [21,22].…”

Section: Introductionmentioning

confidence: 99%

Ionic liquid dynamics in nanoporous carbon: A pore-size- and temperature-dependent neutron spectroscopy study on supercapacitor materials

Busch,

Hofmann,

Frick

et al. 2020

Preprint

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The influence of spatial confinement on the thermally excited stochastic cation dynamics of the room-temperature ionic liquid 1-N-butylpyridinium bis-((trifluoromethyl)sulfonyl)imide ([BuPy][Tf2N]) inside porous carbide-derived carbons with various pore sizes in the sub-to a few nanometer range are investigated by quasi-elastic neutron spectroscopy. Using the potential of fixed window scans, i.e. scanning a sample parameter, while observing solely one specific energy transfer value, an overview of the dynamic landscape within a wide temperature range is obtained. It is shown that already these data provide a quite comprehensive understanding of the confinementinduced alteration of the molecular mobility in comparison to the bulk. A complementary, more detailed analysis of full energy transfer spectra at selected temperatures reveals two translational diffusive processes on different time scales. Both are considerably slower than in the bulk liquid and show a decrease of the respective self-diffusion coefficients with decreasing nanopore size. Different thermal activation energies for molecular self-diffusion in nanoporous carbons with similar pore size indicate the importance of pore morphology on the molecular mobility, beyond the pure degree of confinement. In spite of the dynamic slowing down we can show that the temperature range of the liquid state upon nanoconfinement is remarkably extended to much lower temperatures, which is beneficial for potential technical applications of such systems.

show abstract

Measurement of self-diffusion in thin samples using a novel one-sided NMR magnet

Cited by 9 publications

References 22 publications

Coupling NMR to SANS: Addressing at once structure and dynamics in soft matter

Coupling NMR to SANS: Addressing at once structure and dynamics in soft matter

Ionic liquid dynamics in nanoporous carbon: A pore-size- and temperature-dependent neutron spectroscopy study on supercapacitor materials

Ionic liquid dynamics in nanoporous carbon: A pore-size- and temperature-dependent neutron spectroscopy study on supercapacitor materials

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