In Situ TEM Biasing & Heating

Sample Dynamics
under controlled electrical and thermal environment.

The Lightning In Situ TEM Biasing & Heating Series provides you the power to obtain real-time information about specimen dynamics triggered by temperature and/or electric fields. Investigate the next generation of nano-electronic materials and devices with the Lightning Series.

Lightning Application Fields

Piezoelectrics

ReRam

Solar Cells

Dedicated or simultaneous biasing & heating studies

Nano-scale investigations of nano-electronic devices & materials

E-field induced dynamics of piezoelectric nanoparticle

Experiment: Ba-Sr-Ti-Na-O3 at 800 °C and 210 kV/cm Researchers from TU Darmstadt using the Lightning D9+ (now HB+) JEOL system investigated led free piezoelectric material Ba-Sr-Ti-Na-O3 in the form of nano particles. The nano particles were sintered until a core shell structure formed and a high e-field applied to show domain changes. The in situ TEM video shows through the FFT that the core is ferroelectric and possess domains, however, the shell in paraelectric (non ferroelectric). Showing the superior performance of the Lightning system, high resolution was achieved while applying 210 kV/cm at 800 °C.

Domain evolution in ferroelectric materials

Ferroelectric materials are characterized by the existence of spontaneous electric polarizations at a temperature well below Curie temperature. In a small area, the polarizations may share a same direction and form the so-called ferroelectric domain. The spontaneous polarization can be reversed by applying an external electric field exceeding the coercive field. Investigating the ferroelectric properties at both temperature and external electric field is important for applications such as data storage and optical frequency converters. Here we present a recent experiment performed using the Lightning D9+ (now HB+) demonstrating the capability of delivering both high electric field and stable temperature. Simultaneous electric field and heating is also possible, however, not shown below. The material under investigation is BZT-0.5BCT, which has a Curie temperature around 90 °C and a coercive electric field of 2~4kV/cm.

In Situ TEM Analysis of Organic–Inorganic Metal-Halide Perovskite Solar Cells under Electrical Bias

Abstract Changes in the nanostructure of methylammonium lead iodide (MAPbI3) perovskite solar cells are assessed as a function of current–voltage stimulus by biasing thin samples in situ in a transmission electron microscope. Various degradation pathways are identified both in situ and ex situ, predominantly at the positively biased MAPbI3 interface. Iodide migrates into the positively biased charge transport layer and also volatilizes along with organic species, which triggers the nucleation of PbI2 nanoparticles and voids and hence decreases the cell performance.

Quentin Jeangros*†§, Martial Duchamp‡⊥, Jérémie Werner†, Maximilian Kruth‡, Rafal E. Dunin-Borkowski‡, Bjoern Niesen†, Christophe Ballif†, and Aïcha Hessler-Wyser† † Photovoltaics and Thin-Film Electronics Laboratory, Ecole Polytechnique Fédérale de Lausanne (EPFL), Institute of Microengineering (IMT), Rue de la Maladière 71B, Neuchâtel CH-2000, Switzerland § Department of Physics, University of Basel, Klingelbergstrasse 82, Basel CH-4056, Switzerland ‡ Ernst Ruska—Centre for Microscopy and Spectroscopy with Electrons and Peter Grünberg Institute, Forschungszentrum Jülich D-52425, Germany
nl-2016-03158b_0006

Nano-Chip

Up to 8 contacts for simultaneous biasing & heating

The Lightning Nano-Chips features 4-point-probe method to accurately control biasing and heating and retrieve meaningful data. The design of the Nano-Chip sustains the highest fields and temperatures to be reached (dedicated or simultaneous), enabling the characterization of today’s and tomorrow materials..

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Sample Holder

Introducing the Nano-Chip to the microscope

Made from titanium for its optimal mechanical stability, the Lightning double tilt Sample Holder is the critical element connecting the Nano-Chip with the microscope: designed for the highest flexibility it is compatible with all TEM techniques and features a wide tilt range to be able to look at samples from most orientations.

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Hardware

Total control over the biasing & heating environment

For biasing experiments a source measuring unit (SMU) is required to precisely source voltage or current and simultaneously measure voltage and/or current. The majority of SMUs are compatible with the Lightning system and our preferred supplier/model is Keithley 2450. The Keithley 2450 can conveniently be controlled via the new Impulse SW. Different Keithley models or other can be controlled via the manufacturer’s own software.

Heating experiments are managed via Impulse software.

Impulse software

A seamless integrated system for total control

The new Impulse software provides the user with full control over temperature and electric field. It enables faster experimental setup, easy customization of the workspace and easy monitoring of the experiment

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400 kV/cm @ RT

Biasing

300 kV/cm @ 900 °C

Simultaneous Heating&Biasing

0.6 Å

Resolution

Sample preparation with conventional techniques

The sample preparation techniques used for preparing traditional TEM samples including lamellas, nanowires and particles are suitable for the Nano-Chip. FIB lamellas are the most commonly used sample for biasing experiments and DENSsolutions in conjunction with some close academic partners have developed a unique FIB workflow using a customised FIB stub specifically designed for the Nano-Chip. This process significantly reduces the total workflow time and makes the success in transfer much higher. Additional methods such as micro-manipulators are suitable for sample preparation onto the Nano-Chip.

Some great work from our customers

Testimonials

“Continual advancements of in situ TEM by DENSsolutions provides an exciting and ever-improving level of detail into a range of nano-scale dynamic processes. In particular, the Lightning system allows us to simultaneously heat a FeRh system through magnetic transitions with extreme stability, whilst also applying electrical pulses so that we can drive and visualise magnetic domain wall motion with unparalleled control.” Dr. Trevor Almeida

University of Glasgow

“The ability to apply high electric-fields and to simultaneously perform high-resolution experiments at elevated temperatures is frankly impressive! The new and exciting possibilities that the DENSsolutions Lighting series offers trailblazing new directions at the forefront of materials research.” Dr. Leopold Molina-Luna

Technical University of Darmstadt

“In operando TEM observations provide a unique opportunity to visualise the correlations between the electrical properties and the structural changes. The exceptional stability of the DENSsolutions holder allows the in operando TEM experiments to be performed with atomic resolution. Recently, we successfully observed structural changes of resistive switching and organic-inorganic metal-halide perovskite solar cells devices while under electrical stimulus inside a TEM” Dr. Martial Duchamp

Nanyang Technological University

Frequently Asked Questions

What is the size of sample recommended for biasing experiments?
The sample size depends on the type of experiment to be executed. For 4 point probe measurement approach, where all four biasing electrodes need to be bridged, the required sample length is 10-15 microns. In the situation where only two inner electrodes are involved in the experiment (for example, E-field application), the sample size is can be in the order of 4 microns.
What preparation methods other than FIB could be usable for biasing experiments?
FIB is very important in transferring materials for biasing experiments, especially for lamella’s as it’s the most commonly used method. While for 1D materials (e.g. nanowires) and 2D materials (graphene), the transfer method can vary dependent on what tools you have available such as a micro-manipulator.
What is the homogeneity of the electrical field?
All of our designs show that the uniformity of the electric field is as high as 99%.
What TEM pole-pieces are compatible?
Due to the variety of pole-pieces available for both the JEOL and FEI microscopes, please see the brochure for confirmation. However, the Lightning series is compatible with the smallest pole-pieces found in the JEOL UHR (e.g. ARM) and the FEI Supertwin (e.g. Titan).
What really sets the 50V / 100V limit?

Two reasons:

  1. To avoid the electric failure between connection pins in the vacuum. (Electric sparks)
  2. To avoid breakdown of SiNx at high electric field (the limit is lower at elevated temperature).

Be aware, the specified voltage is not the breakdown voltage of our system, but in fact to ensure a low leakage current. Therefore, in reality one could go much higher than the specified numbers if the experimental details allow.

Can my sample survive the electrical loading induced?
Yes. For common samples, such as lamella’s, metallic nanowires, etc., these samples have proved to be safe during loading without any special care needed. As for sensitive semiconducting nanodevices, grounding connections through source measuring unit / power supply (e.g. Keithley) are needed to make sure there is no static voltage drop over nanodevices, therefore, preventing any damage of high current to the sample.

Download the Lightning Brochure

For more information on features and specifications.

Application Notes


Lightning – In situ TEM Characterization of Electrical Properties of Semiconductor Nanowires

Lightning – In situ atomic-scale observation of electrochemical delithiation in a working solid state battery

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