Search results for "Magic angle"
showing 10 items of 57 documents
Molecular dynamics near the glass transition
1993
Solid state 13C NMR spectroscopy has been applied to investigate the time scale and the geometry of rotational motions near the glass transition of the low-molar-mass van der Waals glass former 1,3,5-tri-α-naphthylbenzene (T g = 342 K). Two-dimensional 13C exchange spectra were taken between 347 and 372 K. With the principal values of the 13C chemical shift tensors determined from 13C CP/MAS spectra and static one-dimensional 13C spectra, the two-dimensional spectra are interpreted according to the isotropic rotational diffusional model to yield mean correlation times τ0 in the range 10 ms ˇ- τ0 ˇ- 50 s, and a log-Gaussian distribution of correlation times with a width of 1·5 decades. The m…
Solid-State NMR, X-ray Diffraction, and Thermoanalytical Studies Towards the Identification, Isolation, and Structural Characterization of Polymorphs…
2009
Combined solid-state NMR, powder, and single crystal X-ray diffraction, as well as thermoanalytical studies were performed towards the identification, isolation, and structural characterization of ...
Mean-field theory for superconductivity in twisted bilayer graphene
2018
Recent experiments show how a bilayer graphene twisted around a certain magic angle becomes superconducting as it is doped into a region with approximate flat bands. We investigate the mean-field $s$-wave superconducting state in such a system and show how the state evolves as the twist angle is tuned, and as a function of the doping level. We argue that part of the experimental findings could well be understood to result from an attractive electron--electron interaction mediated by electron--phonon coupling, but the flat-band nature of the excitation spectrum makes also superconductivity quite unusual. For example, as the flat-band states are highly localized around certain spots in the st…
Effects of nucleotide binding to LmrA: A combined MAS-NMR and solution NMR study
2015
ABC transporters are fascinating examples of fine-tuned molecular machines that use the energy from ATP hydrolysis to translocate a multitude of substrates across biological membranes. While structural details have emerged on many members of this large protein superfamily, a number of functional details are still under debate. High resolution structures yield valuable insights into protein function, but it is the combination of structural, functional and dynamic insights that facilitates a complete understanding of the workings of their complex molecular mechanisms. NMR is a technique well-suited to investigate proteins in atomic resolution while taking their dynamic properties into account…
Non-negative blind source separation techniques for tumor tissue typing using HR-MAS signals.
2010
Given High Resolution Magic Angle Spinning (HR-MAS) signals from several glioblastoma tumor subjects, the goal is to differentiate between tumor tissue types by separating the different sources that contribute to the profile of each spectrum. Blind source separation techniques are applied for obtaining characteristic profiles for necrosis, high cellular tumor and border tumor tissue, and providing the contribution (abundance) of each tumor tissue to the profile of the spectra. The problem is formulated as a non-negative source separation problem. We illustrate the effectiveness of the proposed methods and we analyze to which extent the dimension of the input space could influence the perfor…
Precise measurement of 1H 90° pulse in solid-state NMR spectroscopy for complex and heterogeneous molecular systems
2007
The 90 degrees pulse calibration is essential in NMR spectroscopy to prevent artefacts in the liquid state or to enhance cross-polarization efficiency in the solid state. We verified pulse-angle (PA) errors due to circuit impedances in solid-state NMR and suggested a possible solution to prevent the inconvenience of PA errors. The classic pulse sequences used to calibrate (1)H 90 degrees pulse lengths by direct detection of protons or by cross-polarization were modified in order to replace single (1)H pulses with (1)H pulse trains. Pulse trains were found to decrease the effect of PA imperfections in the calibration of basic pulses (i.e. 90 degrees and 180 degrees ) for a number of organic …
Quantification and classification of high-resolution magic angle spinning data for brain tumor diagnosis.
2007
The goal of this work is to propose a complete protocol (preprocessing, processing and classification) for classifying brain tumors with proton high-resolution magic-angle spinning ((1)H HR-MAS) data. The different steps of the procedure are detailed and discussed. Feature extraction techniques such as peak integration, including also the automated quantitation method AQSES, were combined with linear (LDA) and non-linear (least-squares support vector machine or LS-SVM) classifiers. Classification accuracy was assessed using a stratified random sampling scheme. The results suggest that LS-SVM performs better than LDA while AQSES performs better than the standard peak integration feature extr…
Synthesis and Characterization of SiC/MC/C Ceramics (M = Ti, Zr, Hf) Starting from Totally Non-oxidic Precursors
2002
The reaction of poly(dimethylsilane) (PDMS) and poly(dimethylcarbosilane) (PCS) with bis(cyclopentadienyl)M dichloride Cp2MCl2 (M ) Ti, Zr, Hf) complexes has been used as a new route to obtain ceramic materials based on SiC-containing M. The reaction is completed at a relatively low temperature, 900 °C, yielding the corresponding amorphous SiC/MC ceramics which have been characterized by means of 29 Si MAS NMR. These amorphous materials have been treated at higher temperatures, 1350 °C, under a purified argon atmosphere, yielding partially crystallized products which have been studied by X-ray powder diffraction and 29 Si MAS NMR. The effect of the composition of the mixture of precursors is
H3PW12O40 supported on mesoporous MCM-41 and Al-MCM-41 materials: preparation and characterisation
2011
MCM-41 and Al–MCM-41 has been synthesized using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 °C for 4 h. HPW heteropolyacid supported on the mesoporous were prepared using the incipient wetness method. The characterization of materials was performed by X-ray diffraction, Transmission Electron Microscopy, N2 adsorption, 29Si Cross Polarization–Magic Angle Spinning and 27Al MAS NMR. Results showed that the hexagonal structure is obtained in both cases. The Aluminium species are located inside an extra-framework. The impregnation reduces the surface area of the mesopo…
Low-temperature Ti-containing 3:2 and 2:1 mullite nanocrystals from single-phase gels
2007
Abstract TiO 2 -containig single-phase gels with (Al 2 O 3 + TiO 2 )/(SiO 2 ) molar ratios 3/2 and 2/1 were prepared by gelling mixtures of aluminium nitrate, tetraethylorthosilicate and titanium isopropoxide. Gels were fast heated at several temperatures up to 1100 °C. Dried and heated gels were characterized by differential thermal analysis (DTA), magic angle spinning nuclear magnetic resonance (MAS-NMR), X-ray powder diffraction (XRD), and scanning and transmission electron microscopies (SEM and TEM). Coupled DTA and XRD results of gels fast heated at 900 °C showed the crystallisation of two mullites as well as a small amount of alumina-silica spinel. 27 Al NMR spectra showed the format…