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Nano-segregated soft materials observed by NMR spectroscopy
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry.
2011 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis is about using nuclear magnetic resonance (NMR) spectroscopy for studying soft materials. Soft materials may be encountered everyday by most readers of this thesis, for example when taking a shower or watching TV. The usefulness of these materials originates from them being soft yet, at the same time, having some kind of a structure. The characteristic length scale of those structures is often on the order of nanometers (10-9 m) and the structure can respond to various external stimuli such as temperature, electric and magnetic fields, or the presence of interfaces.

NMR spectroscopy excels when studying soft materials because it is a non-invasive technique with a large spectral resolution. Moreover, different NMR methods allow us to study local molecular dynamics or longer-range translational diffusion. Understanding those latter aspects is very important for the development of dynamic and responsive materials.

Papers I-III present our work on assessing molecular adsorption on interfaces in colloidal dispersions. Here, carbon nanotubes (CNTs) or silica particles were the colloidal substrates to which proteins, polymers or surfactants adsorbed. Papers IV-VI concern ionic mobility in liquid crystals (LCs). The influence of material structure on, for example, the anisotropy of diffusion or on the association/dissociation of ions was studied in several LC phases.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology , 2011. , 46 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 2011:12
Keyword [en]
nuclear magnetic resonance, soft matter, colloidal dispersion, carbon nanotubes, colloidal silica, adsorption, liquid crystals, ionic liquids, diffusion
National Category
Physical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-30337ISBN: 978-91-7415-876-2 (print)OAI: oai:DiVA.org:kth-30337DiVA: diva2:399742
Public defence
2011-03-18, Sal F3, Lindstedtsvägen 26, KTH, Stockholm, 09:30 (English)
Opponent
Supervisors
Note
QC 20110225Available from: 2011-02-25 Created: 2011-02-23 Last updated: 2011-02-25Bibliographically approved
List of papers
1. Protein Dispersant Binding on Nanotubes Studied by NMR Self-Diffusion and Cryo-TEM Techniques
Open this publication in new window or tab >>Protein Dispersant Binding on Nanotubes Studied by NMR Self-Diffusion and Cryo-TEM Techniques
2010 (English)In: JOURNAL OF PHYSICAL CHEMISTRY LETTERS, ISSN 1948-7185, Vol. 1, no 9, 1414-1419 p.Article in journal (Refereed) Published
Abstract [en]

Carbon nanotubes can be dispersed by a variety of molecules. We investigate the dynamics of protein-assisted carbon nanotube dispersion in water. We find that in equilibrium only a small fraction of the dispersants is indeed adsorbed to the nanotube Surface, while there is a fast exchange process between the adsorbed and free protein molecules. Self-diffusion NMR spectroscopy in combination with cryo-transmission electron microscopy imaging are employed.

National Category
Physical Chemistry Materials Engineering Atom and Molecular Physics and Optics Atom and Molecular Physics and Optics
Identifiers
urn:nbn:se:kth:diva-27905 (URN)10.1021/jz100342c (DOI)000277443200024 ()2-s2.0-77952084269 (Scopus ID)
Funder
Swedish Research Council
Note

QC 20110211

Available from: 2011-02-11 Created: 2011-01-03 Last updated: 2016-12-21Bibliographically approved
2. Polymer Binding to Carbon Nanotubes in Aqueous DispersionsStudied by NMR Diffusometry
Open this publication in new window or tab >>Polymer Binding to Carbon Nanotubes in Aqueous DispersionsStudied by NMR Diffusometry
Show others...
(English)Manuscript (preprint) (Other academic)
Abstract [en]

The diffusion behavior of block copolymer Pluronic F-127 in aqueous dispersions of single-walled (SW) and multi-walled (MW) carbon nanotubes (CNT) has been studied by pulsed-field-gradient (PFG) 1H NMR spectroscopy. We show that the polymers are either free monomers or bound to the CNT and exchange between these two states. The residence times and relative populations in those states could also be obtained. For both classes of CNT, the residence time in the bound state was found to be similar and in the order of 10-100 milliseconds. Thermal gravimetric analysis (TGA) showed that the SWCNT concentration dispersed by F-127 was higher than that for MWCNT.

Keyword
Pluronics, F-127, carbon nanotubes, adsorption, residence time, diffusion, nuclear magnetic resonance
National Category
Physical Chemistry
Identifiers
urn:nbn:se:kth:diva-30469 (URN)
Note
QC 20110225Available from: 2011-02-25 Created: 2011-02-25 Last updated: 2011-02-25Bibliographically approved
3. Adsorption isotherms of cationic surfactants on silica particles measured by NMR spectroscopy
Open this publication in new window or tab >>Adsorption isotherms of cationic surfactants on silica particles measured by NMR spectroscopy
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

We present here a new method that employs NMR spectroscopy to quantify the adsorbed amount of surfactant on the surface of particles and thereby provide the adsorption isotherm. As demonstration, the adsorption isotherms for a series of cationic surfactants on silica particles are obtained. Those results are in general agreement with previous observations and the overall appearances of adsorption isotherms exemplify the interplay between electrostatic and hydrophobic interactions. Compared to other available methods, the experimental error is comparable or smaller in a very wide range of surfactant concentrations and there exist other potential advantages.

Identifiers
urn:nbn:se:kth:diva-30471 (URN)
Note
QC 20110225Available from: 2011-02-25 Created: 2011-02-25 Last updated: 2011-02-25Bibliographically approved
4. Ion Channels and Anisotropic Ion Mobility in a Liquid-Crystalline Columnar Phase As Observed by Multinuclear NMR Diffusometry
Open this publication in new window or tab >>Ion Channels and Anisotropic Ion Mobility in a Liquid-Crystalline Columnar Phase As Observed by Multinuclear NMR Diffusometry
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2010 (English)In: Journal of Physical Chemistry B, ISSN 1520-6106, E-ISSN 1520-5207, Vol. 114, no 47, 15477-15482 p.Article in journal (Refereed) Published
Abstract [en]

The anisotropic diffusion of anions and cations in the columnar and isotropic phases of a fan-shaped imidazolium hexafluorophosphate salt is measured by H-1 and F-19 diffusion NMR experiments. The macroscopic orientation of the columnar phase is investigated by H-2 NMR spectroscopy. We find that the anions, confined by the cations, diffuse faster than the cations along the columns but slowly across them, which exemplifies the ion channel model of these materials. The cations and anions are dissociated in the columnar phase but are paired or clustered in the isotropic phase.

Keyword
self-organization, field-gradient, diffusion, water, assemblies, membrane
National Category
Physical Chemistry
Identifiers
urn:nbn:se:kth:diva-27949 (URN)10.1021/jp1082054 (DOI)000284454500007 ()2-s2.0-78649495296 (Scopus ID)
Funder
Swedish Research Council
Note
QC 20110104Available from: 2011-01-04 Created: 2011-01-03 Last updated: 2017-12-11Bibliographically approved
5. Ion conductive behaviour in a confined nanostructure: NMR observation of self-diffusion in a liquid-crystalline bicontinuous cubic phase
Open this publication in new window or tab >>Ion conductive behaviour in a confined nanostructure: NMR observation of self-diffusion in a liquid-crystalline bicontinuous cubic phase
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2010 (English)In: Chemical Communications, ISSN 1359-7345, E-ISSN 1364-548X, Vol. 46, no 5, 728-730 p.Article in journal (Refereed) Published
Abstract [en]

The diffusion of ions in an ionic liquid crystal exhibiting a bicontinuous cubic liquid-crystalline phase has been investigated by NMR spectroscopy in order to examine the behaviour of ions in an ordered nanostructure.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:kth:diva-19170 (URN)10.1039/b915931b (DOI)000274207000017 ()2-s2.0-74549136458 (Scopus ID)
Funder
Swedish Research Council
Note
QC 20110124Available from: 2010-08-05 Created: 2010-08-05 Last updated: 2017-12-12Bibliographically approved
6. Anisotropic Ion Mobility in an Ionic Liquid Crystal Complex of a Rodlike Mesogen Containing an Oxyethylene Moiety and Lithium Triflate
Open this publication in new window or tab >>Anisotropic Ion Mobility in an Ionic Liquid Crystal Complex of a Rodlike Mesogen Containing an Oxyethylene Moiety and Lithium Triflate
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

A liquid-crystalline (LC) complex of a rodlike mesogen containing an oxyethylene moiety and lithium triflate has been synthesized and its mesophases have been characterized by differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD) and polarized optical microscopy (POM). The ion conductive behaviour was investigated in isotropic and LC phases and related to the ionic mobility, as observed by 7Li and 19F NMR diffusometry. The observed two-dimensional ion mobilities show that planes conducting both lithium and triflate ions are formed in the smectic mesophases. The conductivity of the lithium ions is large in the smectic C phase where conductive planes rich in ethylene oxide chains exist.

Identifiers
urn:nbn:se:kth:diva-30473 (URN)
Note

QC 20110225

Available from: 2011-02-25 Created: 2011-02-25 Last updated: 2014-09-24Bibliographically approved

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