In situ

Real-time observation of growth processes, chemical reactions and oxidation, irradiation effects, mechanical, magnetic, and ferroelectric properties.

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Overview: 

Examples of In Situ          Advantages of In Situ

WHAT IS IN SITU?

In-situ transmission electron microscopy (TEM) combines the image formation capabilities of the TEM with the applications of one or more external stimuli to observe real-time sample dynamics. A diverse array of systems and holders allow researchers to apply various stimuli, unlocking the potential to evaluate dynamics during electrical biasing, mechanical strain and deformation, heating, cooling, light illumination, and the introduction of gaseous or liquid environments, as well as intense electron beam irradiation.

Historically, movies of various reactions and system kinetics were recorded on videotape. With the advent of screen capture programs, this process improved, allowing low-resolution, qualitative video capture to visualize what is happening at speeds up to video frame rates, e.g., 30 frames per second (fps).

With advancements in data transfer and processing capabilities, Gatan in-situ cameras can now record and manage large datasets directly from the sensor output. The original quantitative data from each frame captured during an experimental session can be stored directly on disk and treated as individual images or played back as a video.

Additionally, various algorithms or scripts (e.g., summing, drift correction, and binning) can be applied after capture to extract the most useful parts of the acquired data. The free built-in data management tools available for Gatan in-situ cameras allow data to be isolated and extracted easily so that post-processing data analysis can be performed to quantify the observed effects of the stimuli applied to the system.

This streamlined data capture and post-processing workflow significantly increases the probability of acquiring publishable data during a microscopy session. The most advanced in-situ cameras from Gatan offer unprecedented resolution in both time and space, with sub-ms time resolution. This capability allows researchers to study reactions that were previously too fast to capture and resolve previously unknown dynamics.

Today, in-situ electron microscopy encompasses much more than just TEM imaging. Techniques such as scanning transmission electron microscopy (STEM) imaging, diffraction, electron energy loss spectroscopy (EELS), energy-dispersive x-ray spectroscopy (EDS), and 4D STEM can all be acquired continuously while varying stimuli. This allows for deeper insights into the dynamics of the structure, composition, and bonding of materials. Gatan provides the scientific community with tools to apply these techniques to in-situ experiments. Simple in-situ data collection is supported by automatic data synchronization and powerful tools for processing, analysis, and visualization.

EXAMPLES OF IN SITU

The in-situ upgrade to the GIF Continuum® makes in-situ EELS spectrum imaging with real-time quantification of oxidation state, real-time drift correction, and simultaneous EDS and ADF imaging possible. Here, 428 spectrum images were acquired at a rate of 1 every 5 seconds, or about 1 every 2 °C, as the FeOOH sample was heated to 850 °C.

In-situ diffraction video datasets were captured using a Metro® counting camera without any beam stop as the temperature of VO2 oscillated above and below its metal-insulator transition temperature. This video shows the automatically synchronized playback of the original data, the same data after averaging every 10 frames, and the temperature. A linked profile tool is used to visualize better the line of diffraction spots, which only appear at low temperature when the VO2 is insulating.

Low-dose TEM imaging enabled the observation of this beam-induced dendritic growth of Cu. A dose rate of just 1 e-2/s resulted in a growth rate of approximately 10 nm/s. Observation of a 5.7 x 4.1 µm field of view with 0.5 nm pixels was made possible by the K3® IS camera, which captured 11520 x 8184 pixels at 5 fps.

ADVANTAGES OF IN SITU

Capability Advantage
Real-time observation Rapidly collects data from a single sample to understand how materials change.
Environment and stimulus control Captures how different environments and various stimuli can change the structure, properties, and performance of materials.
High spatial and temporal resolution In-situ  TEM can enable spatial resolutions from 10s of nanometers to fractions of an angstrom, plus temporal resolutions from a few seconds to less than a millisecond.
Operando investigation Offers even greater insight when the material's performance and structure are measured during the application of different stimuli.
Variety of techniques Electron microscopy encompasses more than just TEM imaging. It also includes STEM imaging, diffraction, EELS, EDS, and 4D STEM. These techniques can all be acquired continuously while changing stimuli, allowing for a deeper understanding of the dynamics related to the structure, composition, and bonding of materials.

Resources:

 

APPLICATIONS

Crystallization of Sn in various orientations

Crystallization in random orientations monitored via in-situ 4D STEM

High-resolution image of water ice, showing atomic level detail

Atomic resolution imaging of hexagonal water ice

Phase maps generated by MLLS fitting of the O K

The characterization of beam-induced phase changes with in-situ EELS

Ptychographic phase image of Stronium Titrate

K3 IS camera for electron ptychography: Mapping oxygen in SrTiO3

CuO heating results from 100 to 540 ºC, showing copper oxidation state and oxygen ELNES maps produced using standards-based EELS quantification.

Automated in-situ spectrum imaging with synchronized stimulus control

ADF STEM image of the polymer blend and phase map generated using ELNES standards from the C K-edge.

Phase mapping of dose-sensitive polymers using direct detection and multipass in-situ spectrum imaging

Analysis of CaCO3 Particles Using ADF Imaging and EELS Spectroscopy

Dose fractionation using multi-pass in-situ spectrum imaging

High-speed in-situ observation of the annealing of Platinum islands into branched Ruthenium nanostructures

 In-situ observation of the annealing of Pt islands into branched Ru nanostructures to make single-atom catalysts

Sn (Tin) nanoparticle melting and crystallizing as the temperature oscillated

Extensible real-time data processing with Python in DigitalMicrograph

Fourier filtered overlays showing the α (purple) and β (red) phases as the hydrogenation takes place

In-situ lattice-resolution imaging of hydrogen absorption into nanoparticles

Frames showing slow copper dendrite growth

Observing beam-induced dendritic growth over two different timescales

Low-dose in-situ video showing formation of carbon nanoparticles during heating

Imaging carbon nanoparticle agglomeration on MoS2 at a low dose rate

Cryo-TEM image of Li metal filament with SEI

Imaging a lithium metal battery solid electrolyte interphase

Low magnification, low-dose, TEM images of one Molybdenum disulfide grain boundary region before and after biasing to 1 V potential

Electric field-induced structural dynamics in MoS2 observed using in-situ transmission electron microscopy

Graphene imaged at 200 kV

Imaging of graphene at 200 kV using electron counting

Imaging ions at a liquid-solid interface

Imaging discrete ions at a liquid-solid interface using low-dose cryo-EM and electron counting

Schematic of MoS2/hBN sample analyzed

Electric field mapping in 2D heterostructures using differential phase contrast

Lithiation progressed under -6 V of potential, where the Li-ions traveled down the inner wall of the CNT and alloyed with the NiS

Dynamic in-situ lithiation of NiS-filled carbon nanotubes

 Crystallographic grain boundary classification of 2D tellurene

Grain boundary structure of two-dimensional tellurium revealed by 4D STEM

Cu-Sn alloy dissociation acquired with a K3 IS direct detection camera

K3 IS: Low dose EM meets catalysis

 

 

Posters

Continuous EELS Spectrum Imaging of Nano-Droplet Crystallization Heterogeneity

Continuous EELS spectrum imaging of nano-droplet crystallization heterogeneity - EMC 2024

Rapidly analyzing in-situ videos to track lattice spacing

Gigabytes to megabytes – Rapidly analyzing in-situ videos to track lattice spacing - EMC 2024

thermal phase behavior of all-inorganic halide perovskites

Nanoscale insights into the thermal phase behavior of all-inorganic halide perovskites by in-situ 4D STEM - M&M 2024

dose-fractionated spectrum imagingneity

Characterization of beam sensitive samples through dose-fractionated spectrum imaging - MRS Fall 2023

Extensible Real-Time Data Processing

Extensible real-time data processing with Python in DigitalMicrograph - IMC 2023

multipass in-situ spectrum imaging

Dose-fractionated EELS through multipass in-situ spectrum imaging - M&M 2023

heating and multimodal STEM experiments in DigitalMicrogragh

An IR filter for in-situ STEM-EDS heating and multimodal STEM experiments in DigitalMicrogragh - M&M 2023

direct detection camera for transmission electron microscopy imaging

An accessible direct detection camera for transmission electron microscopy imaging, diffraction, & in-situ investigation of materials from 60 – 200 keV - MRS 2022

 
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