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Instruments / Technical Area	Publication Details	Published	Actions
E02-JEM ARM 300CF	Focused-probe STEM ptychography: Developments and opportunities Colum O'Leary , Emanuela Liberti , Gerardo Martinez , Christopher Allen , Chen Huang , Mathias Rothmann , Hui Luo , Judy Kim , Laura Herz , Hazel Assender , Lewys Jones , Angus Kirkland , Peter Nellist Microscopy And Microanalysis Microscopy & Microanalysis 2020 DOI: 10.1017/S1431927620014762 Diamond Proposal Number(s): [20431, 22317]	Jul 2020
I11-High Resolution Powder Diffraction I15-1-X-ray Pair Distribution Function (XPDF)	Interstitial boron atoms in palladium lattice of industrial type of nano-catalyst: Properties and structural modifications Tianyi Chen , Ieuan Ellis , Thomas Hooper , Emanuela Liberti , Lin Ye , Tsz Woon Benedict Lo , Colum O'Leary , Alexandra A. Sheader , Gerardo T. Martinez , Lewys Jones , Ping-Luen Ho , Pu Zhao , James Cookson , Peter T Bishop , Philip A. Chater , John V. Hanna , Peter D. Nellist , Shik Chi Edman Tsang Journal Of The American Chemical Society DOI: 10.1021/jacs.9b06120 Diamond Proposal Number(s): [15452] Show Abstract ▼ Abstract: It is well established that the inclusion of small atomic species such as boron (B) in powder metal catalysts can subtly modify catalytic properties, and the associated changes in the metal lattice implies that the B atoms are located in the interstitial sites. However, there is no compelling evidence for the occurrence of interstitial B atoms, and there is a concomitant lack of detailed structural information describing the nature of this occupancy and its effects on the metal host. In this work, we use an innovative combination of high-resolution 11B magic-angle-spinning (MAS) and 105Pd static solid state NMR nuclear magnetic resonance (NMR), synchrotron X-ray diffraction (SXRD), in-situ X-ray pair distribution function (XPDF), scanning transmission electron microscopy-annular dark field imaging (STEM-ADF), electron ptychography and electron energy loss spectroscopy (EELS) to investigate the B atom positions, properties and structural modifications to the palladium lattice of an industrial type interstitial boron doped palladium nanoparticle catalyst system (Pd-intB/C NPs). In this study we report that upon B incorporation into the Pd lattice, the overall face centered cubic (FCC) lattice is maintained, however short range disorder is introduced. The 105Pd static solid-state NMR illustrates how different types (and levels) of structural strain and disorder are introduced in the nanoparticle history. These structural distortions can lead to the appearance of small amounts of local hexagonal close packed (HCP) structured material in localized regions. The short range lattice tailoring of the Pd framework to accommodate interstitial B dopants in the octahedral sites of the distorted FCC structure can be imaged by electron ptychography. This study describes new toolsets that enables the characterization of industrial metal nanocatalysts across length scales from macro-analysis to micro-analysis, which gives important guidance to structure-activity relationship of the system.	Nov 2019

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E02-JEM ARM 300CF

Focused-probe STEM ptychography: Developments and opportunities

Colum O'Leary , Emanuela Liberti , Gerardo Martinez , Christopher Allen , Chen Huang , Mathias Rothmann , Hui Luo , Judy Kim , Laura Herz , Hazel Assender , Lewys Jones , Angus Kirkland , Peter Nellist

Microscopy And Microanalysis Microscopy & Microanalysis 2020

DOI: 10.1017/S1431927620014762

Diamond Proposal Number(s): [20431, 22317]

Jul 2020

I11-High Resolution Powder Diffraction
I15-1-X-ray Pair Distribution Function (XPDF)

Interstitial boron atoms in palladium lattice of industrial type of nano-catalyst: Properties and structural modifications

Tianyi Chen , Ieuan Ellis , Thomas Hooper , Emanuela Liberti , Lin Ye , Tsz Woon Benedict Lo , Colum O'Leary , Alexandra A. Sheader , Gerardo T. Martinez , Lewys Jones , Ping-Luen Ho , Pu Zhao , James Cookson , Peter T Bishop , Philip A. Chater , John V. Hanna , Peter D. Nellist , Shik Chi Edman Tsang

Journal Of The American Chemical Society

DOI: 10.1021/jacs.9b06120

Diamond Proposal Number(s): [15452]

Show Abstract ▼

Abstract: It is well established that the inclusion of small atomic species such as boron (B) in powder metal catalysts can subtly modify catalytic properties, and the associated changes in the metal lattice implies that the B atoms are located in the interstitial sites. However, there is no compelling evidence for the occurrence of interstitial B atoms, and there is a concomitant lack of detailed structural information describing the nature of this occupancy and its effects on the metal host. In this work, we use an innovative combination of high-resolution 11B magic-angle-spinning (MAS) and 105Pd static solid state NMR nuclear magnetic resonance (NMR), synchrotron X-ray diffraction (SXRD), in-situ X-ray pair distribution function (XPDF), scanning transmission electron microscopy-annular dark field imaging (STEM-ADF), electron ptychography and electron energy loss spectroscopy (EELS) to investigate the B atom positions, properties and structural modifications to the palladium lattice of an industrial type interstitial boron doped palladium nanoparticle catalyst system (Pd-intB/C NPs). In this study we report that upon B incorporation into the Pd lattice, the overall face centered cubic (FCC) lattice is maintained, however short range disorder is introduced. The 105Pd static solid-state NMR illustrates how different types (and levels) of structural strain and disorder are introduced in the nanoparticle history. These structural distortions can lead to the appearance of small amounts of local hexagonal close packed (HCP) structured material in localized regions. The short range lattice tailoring of the Pd framework to accommodate interstitial B dopants in the octahedral sites of the distorted FCC structure can be imaged by electron ptychography. This study describes new toolsets that enables the characterization of industrial metal nanocatalysts across length scales from macro-analysis to micro-analysis, which gives important guidance to structure-activity relationship of the system.

Nov 2019

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