Resolving single Cu nanoparticle oxidation and Kirkendall void formation with <i>in situ</i> plasmonic nanospectroscopy and electrodynamic simulations

Nilsson, Sara; Albinsson, David; Antosiewicz, Tomasz J.; Fritzsche, Joachim; Langhammer, Christoph

doi:10.1039/c9nr07681f

Cited by 39 publications

(55 citation statements)

References 29 publications

(44 reference statements)

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“…3a). The spectral evolution is in very good agreement with a corresponding study of single Cu nanoparticle oxidation by Nilsson et al 39 . By then integrating the scattering intensity over the whole measured wavelength range, the total scattering intensity is found at each time step, and plotted as function of time in Fig.…”

Section: Resultssupporting

confidence: 90%

Copper catalysis at operando conditions—bridging the gap between single nanoparticle probing and catalyst-bed-averaging

et al. 2020

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In catalysis, nanoparticles enable chemical transformations and their structural and chemical fingerprints control activity. To develop understanding of such fingerprints, methods studying catalysts at realistic conditions have proven instrumental. Normally, these methods either probe the catalyst bed with low spatial resolution, thereby averaging out single particle characteristics, or probe an extremely small fraction only, thereby effectively ignoring most of the catalyst. Here, we bridge the gap between these two extremes by introducing highly multiplexed single particle plasmonic nanoimaging of model catalyst beds comprising 1000 nanoparticles, which are integrated in a nanoreactor platform that enables online mass spectroscopy activity measurements. Using the example of CO oxidation over Cu, we reveal how highly local spatial variations in catalyst state dynamics are responsible for contradicting information about catalyst active phase found in the literature, and identify that both surface and bulk oxidation state of a Cu nanoparticle catalyst dynamically mediate its activity.

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Section: Resultssupporting

confidence: 90%

Copper catalysis at operando conditions—bridging the gap between single nanoparticle probing and catalyst-bed-averaging

et al. 2020

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“…The reproducibility of this double masking-based sample preparation method eases the tuning of the sample thickness during direct deposition, which is an important consideration to overcome the geometrical blurring effect [1] in TEM characterization. Henceforth, the discussed procedure may assist future developments such as the fabrication of nanoelectronic devices by in-situ TEM ablation lithography, [9] in-situ oxygen diffusion studies of nano structures, [38] or multicomponent thin film in-situ temperature dependent phase transformation studies. [13] The present masking setup can be successfully used for any type of in-situ TEM sample preparation, including chemical methods.…”

Section: Discussionmentioning

confidence: 99%

Double shadow masking sample preparation method for in‐situ TEM characterization

et al. 2020

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A novel double mechanical masking-based sample preparation method is introduced for in-situ transmission electron microscopy (TEM) characterizations. In the current study amorphous vanadium pentoxide thin film deposition is carried out by using the developed double mask on a transparent window of TEM chip on precisely selected spots by a reactive sputtering technique. The prepared sample is less damaged since it is not subjected to ion beam exposure. And the probability of achieving a viable TEM sample is also enhanced compared to classical preparation methods. In-situ temperature-based electron diffraction pattern sequences are recorded for amorphous vanadium pentoxide in the temperature region of 25 to 500˚C. This allowed observing the crystallization temperature at ∼416˚C. The pre-and post-heat-treated microstructure and electron diffraction pattern of the vanadium pentoxide thin film showed the formation of a mixed crystalline and amorphous film. Thus, a most reliable, reusable and cost effective TEM sample preparation method was demonstrated. K E Y W O R D S amorphous crystalline behavior, double masking techniques, electron diffractions, in-situ transmission electron microscopy, vanadium pentoxide (V 2 O 5) This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited.

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“…3D tomography would allow answering intriguing questions regarding surface structure, as pointed out in a review by Miao and co-workers. 428 Since intermediate characterization is vital in mechanistic studies, it will not be limited to electron microscopy, and we expect other in situ techniques (e.g., X-ray, 429,430 optical spectroscopy [431][432][433][434] ) to gain traction alongside the growing use of multimodal imaging. 435 The integration of hybrid nanostructures in various devices and applications depends tremendously on the progress that is achieved in two directions: simplifying and reducing the synthesis costs and also developing heavy metal-free (abundant and nontoxic elements) and stable hybrid nanostructures; these are yet to emerge.…”

Section: Perspectivementioning

confidence: 99%

Metal/semiconductor interfaces in nanoscale objects: synthesis, emerging properties and applications of hybrid nanostructures

Volokh

Mokari

2020

Nanoscale Adv.

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Resolving single Cu nanoparticle oxidation and Kirkendall void formation with in situ plasmonic nanospectroscopy and electrodynamic simulations

Abstract: Copper nanostructures are ubiquitous in microelectronics and heterogeneous catalysis and their oxidation is a topic of high current interest and broad relevance.

Cited by 39 publications

References 29 publications

Copper catalysis at operando conditions—bridging the gap between single nanoparticle probing and catalyst-bed-averaging

Copper catalysis at operando conditions—bridging the gap between single nanoparticle probing and catalyst-bed-averaging

Double shadow masking sample preparation method for in‐situ TEM characterization

Metal/semiconductor interfaces in nanoscale objects: synthesis, emerging properties and applications of hybrid nanostructures

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