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HiGH AND VERY HIGH TEMPERATURE NMR SPECTROSCOPY OF INORGANIC SOLIDS AND LIQUIDS : STRUCTURE, DYNAMICS

Objective



Optimisation of the properties of materials whose fabrication process requires a high temperature liquid step is strongly dependent on our microscopic knowledge of the liquid state and on cooling/solidification mechanisms. Spectroscopic methods are the most likely to provide this knowledge. Their success will depend on the performance of the technique at temperature (general rule: decreasing signal/noise ratio with rising temperature), together with general high temperature science problems such as chemical interaction between the sample and its container and the reliability of the temperature measurements. Nuclear magnetic resonance is the only spectroscopy offering local structural and dynamic information at high temperature. The high and very high temperature probes developed at the Centre de Recherches sur la Physique des Hautes Temperatures (CNRS), the complementary high temperature science facilities and state of the art spectrometers devoted to high temperature NMR work, operated by highly trained and internationally recognised scientists together offer unique opportunities in the following areas:
1. Structural and dynamic studies of non metallic liquids by multinuclear NMR spectroscopy. Atmospheric control (oxidizing, neutral or reducing), contactless conditions and time resolved experiments allow the analysis of a large range of kinetic or cooling processes in the 1300 - 2500rC range. 2. Structural and dynamic studies of solids and liquids up to 1400rC with full multi-nuclear capability in probes with sample containers. 3. The study of phase transitions in crystalline materials and the in situ observation of the transformation to the crystalline state of amorphous materials (e.g. sol-gel derived) or glasses using high temperature static and/or Magic Angle Spinning (MAS) probes. The two different magnetic fields are invaluable for studies of quadrupolar nuclei (e.g. 17 O, 27 Al, 25Mg). 4. NMR experiments are supported by on the site thermal analysis characterization in contactless conditions (or in classic crucible devices), classical high temperature X-Ray experiments. A 'soft' (chimie douce) chemistry laboratory with well developed protocols to allow researchers to prepare isotopically enriched materials ( 17 O for example).

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Coordinator

Centre National de la Recherche Scientifique (CNRS)
EU contribution
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Address
1d avenue de la Recherche Scientifique
45071 Orléans
France

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