Phase Transformations in Porous Materials Studied by in Situ Solid-State NMR Spectroscopy and in Situ X-ray Diffraction

Paula C, Wisser D, Rangus M, Schwieger W, Hovestadt M, Kriesten M, Vanatalu K, Oss A, Org ML, Samoson A, Hartmann M (2020)

Publication Type: Journal article

Publication year: 2020

Journal

Journal of Physical Chemistry C American Chemical Society

Book Volume: 124

Pages Range: 19136-19145

Journal Issue: 35

DOI: 10.1021/acs.jpcc.0c05921

Abstract

Studying complex processes in solid phases such as adsorption or phase transitions in situ is the best way to obtain detailed and realistic insights on a molecular level. Besides in situ X-ray diffraction techniques, magic angle spinning (MAS) solid-state NMR spectroscopy is one of the most powerful analytical techniques. The implementation of in situ and operando MAS NMR is however challenging and requires dedicated hardware. We introduce here a new 4.0 mm wide-bore probe that allows for a continuous and well-distributed flow of gaseous adsorbates or reactants through the packed sample, as well as uniform heating of the sample and spinning of the rotor at the magic angle. The combination of both in situ MAS NMR and in situ powder X-ray diffraction allowed us to obtain new insights into two phase transformation mechanisms in crystalline, porous materials, viz. that of aluminophosphate VPI-5 into AlPO4-8 and that of metal-organic frameworks from the MIL-53 family during water adsorption and desorption.

Authors with CRIS profile

Carolin Paula Interdisziplinäres Zentrum Erlangen Catalysis Resource Center (ECRC) Dorothea Wisser Interdisziplinäres Zentrum Erlangen Catalysis Resource Center (ECRC) Mojca Rangus Interdisziplinäres Zentrum Erlangen Catalysis Resource Center (ECRC) Wilhelm Schwieger Professur für Technische Chemie (Reaktionstechnik) Maximilian Hovestadt Interdisziplinäres Zentrum Erlangen Catalysis Resource Center (ECRC) Martin Kriesten Interdisziplinäres Zentrum Erlangen Catalysis Resource Center (ECRC) Martin Hartmann Professur für Katalyse

Involved external institutions

Tallinn University of Technology EE Estonia (EE)

How to cite

APA:

Paula, C., Wisser, D., Rangus, M., Schwieger, W., Hovestadt, M., Kriesten, M.,... Hartmann, M. (2020). Phase Transformations in Porous Materials Studied by in Situ Solid-State NMR Spectroscopy and in Situ X-ray Diffraction. Journal of Physical Chemistry C, 124(35), 19136-19145. https://dx.doi.org/10.1021/acs.jpcc.0c05921

MLA:

Paula, Carolin, et al. "Phase Transformations in Porous Materials Studied by in Situ Solid-State NMR Spectroscopy and in Situ X-ray Diffraction." Journal of Physical Chemistry C 124.35 (2020): 19136-19145.

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