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Dynamic in-situ microscopy relating structure and function

Discussion meeting

Location

The Royal Society, London, 6-9 Carlton House Terrace, London, SW1Y 5AG

Overview

Fast-track discussion meeting organised by Dame Pratibha Gai FREng FRS, Professor Edward Boyes, Professor Rik Brydson and Professor Richard Catlow FRS.

Atomic level dynamics of irregular nano-gold: by Gai, Boyes and group

This meeting will evidence and advance development in dynamic in-situ environmental electron, scanning probe, optical and fast time resolved microscopy and computer modelling studies of vital interest in the chemical, physical and life sciences, underpinning technologies of high commercial and societal value. It will focus on the pivotal role of imaging and spectroscopy for dynamic processes across the sciences to access previously invisible aspects of real world processes.

The schedule of talks and speaker biographies are available below. Speaker abstracts are also available below. Recorded audio of the presentations will be available on this page after the meeting has taken place. 

Attending the event

This meeting is intended for researchers in relevant fields.

  • Free to attend
  • Limited places, advance registration essential
  • An optional lunch can be purchased during registration

Enquiries: contact the Scientific Programmes team

Event organisers

Select an organiser for more information

Schedule of talks

21 October

09:00-12:30

Session 1

6 talks Show detail Hide detail

Chairs

Professor Dame Pratibha Gai FREng FRS, University of York, UK

09:00-09:30 Native state analysis of complex, beam-sensitive systems by electron microscopy

Professor Rik Brydson, University of Leeds, UK

Abstract

Complex, electron-beam sensitive systems include organic crystals, hybrid organic-inorganic materials, some inorganic materials such as hydrates as well as multiphase solid/liquid and solid/gas materials. Arguably they constitute the majority of systems of current interest across a wide range of scientific and engineering disciplines including chemistry and chemical engineering, engineering materials, food science, biology and increasingly physics and electronic engineering.

For the purposes of this presentation Professor Brydson defines in-situ as the native-state analysis of such complex, beam sensitive materials and systems, in that they remain unmodified by interaction with the electron beam which is well-known to alter both the structure and chemistry of the specimen. Here, he also concentrates almost exclusively on transmission electron microscopy (TEM) of thin specimens. 

Electron dose is related to the energy absorbed by the specimen during electron irradiation and can be a function of both the electron fluence and fluence rate in the TEM. Professor Brydson discusses a number of useful concepts for TEM imaging and/or chemical analysis, including a dose budget for experiments and also a dose-limited resolution. We also highlight the current state-of-the-art in dose control during imaging and spectroscopy including the use of scanning TEM (STEM) as opposed to conventional TEM (CTEM), compressed sensing methods and the cryo-preservation of samples.

Finally, he also discusses dynamic studies of such complex materials and systems including the use of in-situ liquid and gas cells TEM holders, which have their own additional limitations due to dose, as well as the use of time-resolved cryo-methods to provide snapshots of dynamic systems.

 

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09:30-09:40 Discussion

09:40-10:10 Spatio-temporal dynamics of active catalysts observed by multi-scale in-situ electron microscopy

Dr Marc Willinger, ETH Zürich, Switzerland

Abstract

Catalysts are operating far from thermodynamic equilibrium in an open system that exchanges heat and matter with the surrounding. In their active state, they are supposed to repeatably facilitate sequences of reaction steps of a catalytic cycle. The combination of non-equilibrium conditions and cyclic behaviour can result in complex dynamics and formation of dissipative structures. Such structures are difficult to study because they only exist under reactive conditions. Furthermore, they are difficult to predict using computational methods because of the non-linearity of the underlying kinetics. Structure-function relationships have thus to be studied under relevant reaction conditions. While in situ TEM enables observation of atomistic details under conditions of slow kinetics, in situ SEM delivers complementary information about catalyst dynamics at reduced lateral resolution and provides insight about collective phenomena that are controlled by heat and mass transport. As will be shown in the presentation, the combination of in situ SEM with in situ TEM enables a multi-scale approach for the study of catalyst dynamics from the Å to the mm range and across pressures ranging from 10-5 to 10+5 Pa. Combined with simultaneous detection of reaction products by RGA it is possible to correlate structural dynamics with catalytic activity.

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10:10-10:20 Discussion

10:20-10:50 Coffee

10:50-11:20 Using light to see at the atomic scale using pico-cavities

Professor Jeremy J Baumberg FRS, University of Cambridge, UK

Abstract

Recent advances in using noble metals to confine light to the sub-nm3 scale through advanced plasmonics is opening up a new realm of 'picoscopy'. Professor Baumberg will show how a wide range of dynamic motions of atoms and molecules can be studied on microsecond timescales under ambient conditions. This explores crucial realms of catalytic surface reconstructions and electrochemical interfaces that have been inaccessible.

Professor Baumberg will show how simple nano-architectures enable such trapping of visible light, and how elastic and inelastic light scattering reveal detailed spectral information about extremely small volumes of space. A few examples will highlight the light-induced motion of individual gold atoms, of flickering defects in metal interfaces, and of individual bonds in single molecules moving in real time.

 

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11:20-11:30 Discussion

11:30-12:00 The Light Years: combined optical and environmental electron microscopy to visualise plasmonic processes with atomic-scale resolution

Professor Jennifer Dionne, Stanford University, USA

Abstract

Pearl Jam’s hit, 'The Light Years', declares "We were but stones, light made us stars". Bringing light to the transmission electron microscope (TEM) promises to transform our understanding of materials, enabling both direct observation of light-mediated processes and detection of optical emission with atomic scale resolution. To help achieve this goal, Professor Dionne's lab is developing capabilities for concurrent optical and electron microscopy within an environmental TEM. This presentation will describe their efforts to visualise a variety of plasmonic processes in situ with nanometre-to-atomic scale resolution. The group focuses in particular on i) observing plasmon-driven chemical transformations in nanoparticles; ii) detecting quantum light emission from two-dimensional materials; and iii) developing TEM-Raman with nanometre-scale resolution. First, they study the photocatalytic dehydrogenation of Au-Pd systems, in which the Au acts as a plasmonic light absorber and Pd serves as the catalyst. They find that plasmons modify the rate of distinct reaction steps differently, increasing the overall rate more than ten-fold. Plasmons also open a new reaction pathway that is not observed without illumination, laying a foundation for site-selective and product-specific photocatalysts. Secondly, the group uses scanning transmission electron microscopy and cathodoluminescence spectroscopy to investigate colour centres in two-dimensional hexagonal boron nitride, a wide bandgap material capable of room-temperature, high-brightness visible quantum emission. They find that sharp, single-photon emission peaks are usually associated with regions of multiple fork dislocations, facilitating design of next-generation two-dimensional materials and devices. Finally, they describe a new technique for high-resolution spectroscopy in the TEM: electron-and-light-induced stimulated Raman scattering (ELISR). In particular, theyleverage the electron beam as a highly-localised Angstrom-scale source to locally excite the plasmonic resonances of individual nanoparticles, which stimulate local Raman scattering. They show how ELISR can be used to map molecular signatures with nanometre-scale resolution. 

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12:00-12:10 Discussion

12:10-12:25 Contributed talk

12:25-12:30 Discussion

12:30-13:30 Lunch

13:30-18:00

Session 2

6 talks Show detail Hide detail

Chairs

Professor Jennifer Dionne, Stanford University, USA

Professor Peter van Aken, Max Planck Institute for Solid State Research, Germany

13:30-14:00 Present status and future prospects of environmental HVEM for nanomaterials

Professor Nobuo Tanaka, Nagoya University, Japan

Abstract

Environmental transmission electron microscopy (E-TEM) attracts a strong interest of materials scientists, particularly, those of batteries and catalysts, because the actual chemical reaction processes in gases and liquids should be clarified in real space and in atomic level. E-TEM observations of thick samples also become important for cutting-edge materials in practical use. 3D observation is also necessary for clarifying morphologies of practical catalysts.

Professor Tanaka and colleagues have developed 1MV TEM/STEM equipped with an open-type environmental cell which enables observations in 100 Torr of hydrogen, oxygen, nitrogen and carbon mono-oxide(CO) gases, named 'Reaction Science HVEM'(RSHVEM).

In this talk, Professor Tanaka would like to present new data obtained by the instrument such as (1) in-situ observation of porous gold catalysts, whose inner surfaces with zigzag atom arrangement enhance oxidation of CO gas, (2) observation of diesel soot oxidized in air, and (3) in-situ observation of fractures related to 'hydrogen brittleness' for a Cu/Si interface and  grain boundaries in Ni3Al alloys. Observation of lithium battery materials is also available using a non-exposure transfer holder as well as QMAS ability. Finally, advantages and future prospects of E-HVEM are discussed.

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14:00-14:10 Discussion

14:10-14:35 Atoms in action for energy, healthcare and environment using atomic resolution environmental (S)TEM: advancing the frontiers of chemical research

Professor Dame Pratibha Gai FREng FRS, University of York, UK

Abstract

Many heterogeneous chemical reactions utilise gas-solid catalyst reactions at elevated temperatures and they play a pivotal role in the production of energy, healthcare, pollution control and food. The dynamic catalytic chemical reactions take place at the atom level. Understanding atomic structure evolution and the ensuing catalyst function are vital to developing novel materials and improved chemical processes. However due to limitations of the instrumentation these atomic processes were not well understood. The development of the first atomic resolution-Environmental Transmission Electron Microscope (atomic resolution-ETEM) [Boyes and Gai, Ultramicroscopy 67 (1997) 197], enables the visualisation and analysis of gas-solid catalyst reactions at the atomic level leading to key discoveries and the development is used globally. The ETEM has been advanced to analytical environmental scanning TEM (ESTEM) with single atom resolution and full analytical capabilities. Novel E(S)TEM imaging and analysis in real-time in controlled real-world reaction environments reveal single atom dynamics in fuel cell catalysts, fuels including sustainable biofuels, healthcare applications and ammonia synthesis for agricultural products in food production. The development of a liquid holder enables imaging and analysis of chemical reactions in liquid environments. The dynamic studies, in combination with chemical methods, provide unique insights into atoms in action and atomic scale reaction pathways in chemical reactions, opening new opportunities for the control of the dynamic atomic structure for beneficial catalytic and functional properties. Smarter synthesis leading to improved materials and processes with significantly enhanced performance are possible. Benefits include new knowledge and cleaner processes for renewable energy and healthcare as well as improved or replacement mainstream technologies in the chemical and energy industries.

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14:35-14:40 Discussion

14:40-15:10 Seeing is believing: atomic-scale imaging of catalysts under reaction conditions

Professor Irene Groot, Leiden University, The Netherlands

Abstract

The atomic-scale structure of a catalyst under reaction conditions determines its activity, selectivity, and stability. Recently it has become clear that essential differences can exist between the behaviour of catalysts under industrial conditions (high pressure and temperature) and the (ultra)high vacuum conditions of traditional laboratory experiments. Differences in structure, composition, reaction mechanism, activity, and selectivity have been observed. These observations made it clear that meaningful results can only be obtained at high pressures and temperatures. Therefore, the last years have seen a tremendous effort in designing new instruments and adapting existing ones to be able to investigate catalysts in situ under industrially relevant conditions.

In this talk, Professor Groot will give an overview of the in situ imaging techniques the group uses to study the structure of model catalysts under atmospheric pressures and elevated temperatures. The group has developed set-ups that combine an ultrahigh vacuum environment for model catalyst preparation and characterisation with a high-pressure flow reactor cell, integrated with either a scanning tunneling microscope or an atomic force microscope. With these set-ups the group is able to perform atomic-scale investigations of well-defined model catalysts under industrial conditions. Additionally, they combine the structural information from scanning probe microscopy with mass spectrometry measurements. In this way, the group can correlate structural changes of the catalyst due to the gas composition with its catalytic performance. Furthermore, they use other in situ imaging techniques such as transmission electron microscopy, surface X-ray diffraction, and optical microscopy, all combined with mass spectrometry.

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15:10-15:20 Discussion

15:20-15:40 Coffee

15:40-16:10 Micro to macro-scopic in vivo imaging including magnetic resonance imaging: using advanced medical imaging technologies as a ‘macroscope’ to determine pathophysiologies of complex human brain diseases

Professor Joanna Wardlaw CBE FMedSci, University of Edinburgh and NHS Lothian, UK

Abstract

The rapid advances in understanding and treatment of common human brain diseases have (arguably) been made possible by advances in development of in vivo diagnostic imaging technologies in the last few decades. The human brain is complex, with no truly comparable model species, limiting the ultimate clinical value of many rodent models. Advances in non-invasive medical imaging technologies particularly magnetic resonance imaging, mean that detailed data on brain structure and function and pathological changes in disease can now be determined and tracked in large human samples including population studies and disease cohorts. However, these methods also have limitations of resolution, and tissue often only becomes available post mortem, reflecting end stage disease. Hence, to tackle a complex disorder that develops insidiously in life requires a multimodal approach that includes in vivo MRI and related ‘macroscopic’ methods in patients and volunteers, and parallel and complementary microscopic methods applied to post-mortem brain tissue and in vivo and in vitro static and dynamic imaging methods in rodent models such as MRI, 2-PI, histological and electron microscopic methods. This lecture will illustrate these principles using the example of cerebral small vessel disease, a major cause of both stroke and dementia and of ageing-related multimorbidities.

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16:10-16:20 Discussion

16:20-16:50 Modelling the structures of crystals and nano-particles

Professor Richard Catlow FRS, University College London, UK

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16:50-17:00 Discussion

17:00-18:00 Poster session

22 October

09:00-12:30

Session 3

6 talks Show detail Hide detail

Chairs

Professor Archie Howie CBE FRS, University of Cambridge, UK

09:00-09:30 Molecular to cellular mechanics probed by high-speed atomic force microscopy

Professor Felix Rico, U1067 Aix-Marseille University, CNRS and Inserm, France

Abstract

Mechanical forces in biological processes operate at the level of individual proteins, macromolecular complexes and the whole cell. Moreover, the dynamic response of biological processes span over several orders of magnitude in time, from sub-microseconds to several minutes. Thus, deciphering the role of mechanical forces in biological systems requires probing their mechanical properties over a wide range of length and time scales. High-speed atomic force microscopy (HS-AFM) is a unique technology allowing sub-second, nanometric imaging. Professor Rico's group has adapted HS-AFM to perform high-speed force spectroscopy (HS-FS) both on single molecules and living cells with microsecond time resolution. They probed protein unfolding and receptor/ligand unbinding up to the velocity of molecular dynamics simulations. HS-FS gives access to previously hidden events and, combined with MD simulations, provides atomistic understanding of biomolecular processes based on experimental results. These recent results revealed heterogeneous and rate dependent unfolding and unbinding pathways on different biomolecules. At the cellular level, the group has developed high-frequency microrheology to probe the mechanics of cells at short timescales, down to ~10 µs. The group probed the viscoelastic response of different cell types and upon cytoskeleton perturbation. At microsecond timescales, cells exhibit rich viscoelastic responses that depend on the state of the cytoskeleton and on the cell type. Mechanical measurements over a wide dynamic range provides a mechanistic understanding of cell mechanics based on the dynamics of individual filaments. Thus, HS-FS opens an avenue to better understand the dynamics of proteins and cells at previously inaccessible short timescales.

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09:30-09:40 Discussion

09:40-09:55 Contributed talk

09:55-10:00 Discussion

10:00-10:30 Emerging imaging technologies to study cell architecture, dynamics and function

Professor Jennifer Lippincott-Schwartz, Howard Hughes Medical Institute, USA

Abstract

Powerful new ways to image the internal structures and complex dynamics of cells are revolutionising cell biology and bio-medical research. Here, Professor Lippincott-Schwartz will focus on how emerging fluorescent technologies are increasing spatio-temporal resolution dramatically, permitting simultaneous multispectral imaging of multiple cellular components. Using these tools, it is now possible to begin constructing an 'organelle interactome' describing the interrelationships of different cellular organelles as they carry out critical functions. The same tools are also revealing how genetic mutations disrupting these organelles underlie various human diseases.

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10:30-10:40 Discussion

10:40-11:10 Coffee

11:10-11:40 Radiation damage in electron images of biological structures

Professor Richard Henderson CH FMedSci FRS, MRC Laboratory of Molecular Biology, UK

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11:40-11:50 Discussion

11:50-12:05 Contributed talk

12:05-12:10 Discussion

12:10-12:25 Contributed talk

12:25-12:30 Discussion

12:30-13:30 Lunch

13:30-17:00

Session 4

6 talks Show detail Hide detail

Chairs

Sir Colin Humphreys CBE FREng FRS, Queen Mary University of London, UK

13:30-14:00 Far-field radiation of three-dimensional plasmonic gold tapers and of dynamic toroidal moments

Professor Peter van Aken, Max Planck Institute for Solid State Research, Germany

Abstract

Elementary electromagnetic sources with well-defined near- and far-field properties form the fundamentals to systematically describe and understand observed electromagnetic phenomena of nanometre-sized objects, as well as their interactions and potential applications. Electron energy-loss spectroscopy (EELS) and cathodoluminescence spectroscopy (CL) can access these optical properties at nanometre spatial resolution, where the contrasting juxtaposition of EELS and CL information on the identical object helps to discern radiative from non-radiative optical modes.

This presentation will exemplify the applications of both EELS and CL for enhancing the perception in nano-optics by showing two case studies, namely the far-field radiation of three-dimensional plasmonic gold taper and of dynamic toroidal moments. The studies on the gold tapers revealed that the excited surface plasmons either are guided away from the apex along the taper or couple to the far-field radiation depending on the tapers’ opening angle. The radiative nature of dynamic toroidal dipole modes supported in oligomer nanocavities in thin silver films has been addressed to distinguish them from static toroidal dipoles and plasmonic dark modes. Moreover, numerical finite-difference time-domain simulations were performed for comprehensive understanding and strengthening the conclusions.

This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No. 823717 – ESTEEM3.

 

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14:00-14:10 Discussion

14:10-14:40 Opportunities and challenges in Environmental Scanning Transmission Electron Microscopy (ESTEM) for gas reaction catalysis

Professor Edward D Boyes, University of York, UK

Abstract

Heterogeneous gas-solid catalysis depends on interactions down to single atoms, separately or in ensemble, with selected parts of gas molecules. The ESTEM has been developed to provide atom-by-atom levels of sensitivity and context in catalyst analysis. The preparation, transfer, operation and analysis of meaningful chemically active catalytic surfaces all need to be under controlled conditions of continuous gas atmosphere and temperature, rather than using a standard high vacuum instrument after transfer of sensitive surfaces through air from a conventional chemical reactor. The ESTEM supports dynamic in-situ reaction studies in a custom designed instrument combining reaction chemistry with uncompromised analysis, including (heavier) single atom resolution STEM. It supports fundamental studies of the key processes of activation, reaction, deactivation and reactivation, by combining continuous chemical reaction capabilities with minimally invasive full function single atom resolution STEM. The presentation includes reports of activation, structurally selective reaction, deactivation and reactivation mechanisms, together with discussion of the contribution the method can make to the underlying science and management of catalytic reactions for societal good, including in emission controls and the energy sector.

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14:40-14:45 Discussion

14:45-15:00 Contributed talk

15:00-15:05 Discussion

15:05-15:30 Coffee

15:30-16:00 Femtosecond TEM: status, challenges and outlook

Professor David J Flannigan, University of Minnesota, USA

Abstract

Using an ultrashort-pulsed laser to both trigger specimen excitation in situ and to generate discrete packets of photoelectrons in the TEM gun region enables temporal resolutions to be extended to femtosecond timescales. Such an approach – dubbed ultrafast electron microscopy (UEM) – has been explored in earnest for the last 15 years, and the number of operational systems has steadily increased over this time. Though still somewhat lacking and system dependent, benchmarking generally has shown that coherence can be retained within a particular parameter space, resulting in spatial and energy resolutions that are on par with those achievable with the conventional instrument. Accordingly, numerous discoveries and paradigm tests have been reported, including (for example) the direct visualisation of acoustic-phonon dynamics in plasmonic metallic nanocrystals and archetypal semiconducting materials. Despite noteworthy advances, significant challenges remain with respect to combined spatiotemporal resolutions, accessible fundamental phenomena, and practical ease of use. Here, Professor Flannigan will provide an overview of the current status of UEM instrumentation and capabilities, illustrated in part with specific examples detailing femtosecond bright-field imaging of coherent structural dynamics. He will then outline and describe challenges and limitations of the current approaches, particularly from the perspective of a materials scientist. This will include a discussion of the importance of balancing instrument repetition rate with specimen recoverability and spatiotemporal resolution. Finally, he will conclude with a discussion of the promising new approaches being pursued, and I will share my perspective on the outlook of the field.

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16:00-16:10 Discussion

16:10-16:25 Contributed talk

16:25-16:30 Discussion

16:30-17:00 Panel discussion

Dynamic in-situ microscopy relating structure and function

21 - 22 October 2019

The Royal Society, London 6-9 Carlton House Terrace London SW1Y 5AG UK
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