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Direct solid state NMR observation of the 105Pd nucleus in inorganic compounds and palladium metal systems

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Hooper, Thomas J. N., Partridge, Thomas A., Rees, Gregory J., Keeble, Dean S., Powell, Nigel A., Smith, Mark E., Mikheenko, Iryna P., Macaskie, Lynne E., Bishop, Peter T. and Hanna, John V. (2018) Direct solid state NMR observation of the 105Pd nucleus in inorganic compounds and palladium metal systems. Physical Chemistry Chemical Physics, 20 (41). pp. 26734-26743. doi:10.1039/c8cp02594k

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Official URL: http://dx.doi.org/10.1039/c8cp02594k

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Abstract

The ability to clearly relate local structure to function is desirable for many catalytically relevant Pd-containing systems. This report represents the first direct 105Pd solid state NMR measurements of diamagnetic inorganic (K2Pd(IV)Cl6, (NH4)2Pd(IV)Cl6 and K2Pd(IV)Br6) complexes, and micron- and nano-sized Pd metal particles at room temperature, thereby introducing effective 105Pd chemical shift and Knight shift ranges in the solid state. The very large 105Pd quadrupole moment (Q) makes the quadrupole parameters (CQ, ηQ) extremely sensitive to small structural distortions. Despite the well-defined high symmetry octahedral positions describing the immediate Pd coordination environment, 105Pd NMR measurements can detect longer range disorder and anisotropic motion in the interstitial positions. The approach adopted here combines high resolution X-ray pair distribution function (PDF) analyses with 105Pd, 39K and 35Cl MAS NMR, and shows solid state NMR to be a very sensitive probe of short range structural perturbations. Solid state 105Pd NMR observations of ∼44–149 μm Pd sponge, ∼20–150 nm Pd black nanoparticles, highly monodisperse 16 ± 3 nm PVP-stabilised Pd nanoparticles, and highly polydisperse ∼2–1100 nm biomineralized Pd nanoparticles (bio-Pd) on pyrolysed amorphous carbon detect physical differences between these systems based on relative bulk:surface ratios and monodispersity/size homogeneity. This introduces the possibility of utilizing solid state NMR to help elucidate the structure–function properties of commercial Pd-based catalyst systems.

Item Type: Journal Article
Subjects: Q Science > QD Chemistry
Divisions: Faculty of Science > Physics
Library of Congress Subject Headings (LCSH): Inorganic compounds, Palladium
Journal or Publication Title: Physical Chemistry Chemical Physics
Publisher: Royal Society of Chemistry
ISSN: 1463-9076
Official Date: 7 November 2018
Dates:
DateEvent
7 November 2018Published
31 August 2018Available
31 August 2018Accepted
Volume: 20
Number: 41
Page Range: pp. 26734-26743
DOI: 10.1039/c8cp02594k
Status: Peer Reviewed
Publication Status: Published
Access rights to Published version: Open Access
Funder: awm
RIOXX Funder/Project Grant:
Project/Grant IDRIOXX Funder NameFunder ID
EP/P511432/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
UNSPECIFIEDJohnson Matthey Plchttp://viaf.org/viaf/122487478
UNSPECIFIEDUniversity of Warwickhttp://dx.doi.org/10.13039/501100000741
Advanced Materials Project 1: Creating and Characterising Next Generation Advanced MaterialsBirmingham Science CityUNSPECIFIED
UNSPECIFIEDAdvantage West Midlands (AWM)UNSPECIFIED
UNSPECIFIED[ERDF] European Regional Development Fundhttp://dx.doi.org/10.13039/501100008530
UNSPECIFIED[BBSRC] Biotechnology and Biological Sciences Research Councilhttp://dx.doi.org/10.13039/501100000268
Advanced Materials Projects 2Birmingham Science CityUNSPECIFIED

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