An interview with Product Manager Dr. Gin Pivak about our latest In Situ TKD Stage

DENSsolutions introduces its latest solution for electron microscopy: the In Situ TKD Stage. This stage allows you to perform high resolution microstructural characterization inside your SEM using Transmission Kikuchi Diffraction (TKD) while heating or biasing your sample. We interviewed our Product Manager Dr. Gin Pivak to learn all about the stage, from the reason behind its development to its innovative capabilities. 

Why was this In Situ TKD Stage designed?

The electron backscatter diffraction method (EBSD) has been widely used to study crystal orientation, phase identification and grain size distribution in steels and other types of materials. However, the resolution of the EBSD technique is limited at best to 20 nm, allowing you to characterize polycrystalline materials down to about 100 nm in grain size. To attain a higher resolution, users must resort to transmission electron microscopes (TEM), 4D STEM and/or converging beam electron diffraction (CBED) methods, which are much less accessible.

The TKD method, on the other hand, enables orientation maps of electron transparent samples and allows you to quantitatively map changes in crystal orientation or structure in nanocrystalline materials. Moreover, the TKD experiment can be performed in a SEM, making the technique considerably more accessible with a shorter set-up time and lower cost of entry compared to that of TEM.

DENSsolutions realizes the challenges users are facing in regards to technical limitations, accessibility, time and costs. The In Situ TKD stage was therefore developed, enabling in situ studies of grain distribution and orientation maps of fine-grained and heavily deformed materials. It allows you to have a high spatial resolution similar to that of a TEM but without its impediments. The in situ TKD stage can be used in various applications fields such as automotive, aerospace, electronics, and power generation where in situ heating and/or biasing can help to understand and improve the properties of materials and devices.

What are the main benefits of the In Situ TKD Stage?

One of the most important benefits that the TKD Stage offers as a result of its unique geometry is its ability to perform microstructural characterization using the TKD method with high spatial resolution and simplified grain orientation mapping in SEM under in situ heating and/or biasing stimuli. It also allows you to save valuable time on the TEM as you can perform quick preliminary in situ sample characterization inside the SEM instead and to simplify a correlative analysis. Moreover, with the TKD Stage you can conduct a complete range of in situ heating and/or biasing experiments inside the SEM without the need of accessing a TEM.

to save you valuable time on the TEM, as you can perform quick preliminary in situ sample characterization inside the SEM instead. Moreover, with the TKD Stage you can conduct in situ heating and/or biasing experiments inside the SEM, making it considerably more accessible for users who are unable to access a TEM. Furthermore, as a result of its unique geometry, the In Situ TKD Stage allows you to perform microstructural characterization using the TKD method with high spatial resolution and simplified grain orientation mapping. 

The stage also allows you to easily interchange your chips as it is fully compatible with all double-tilt Wildfire and Lightning chips. Because of this, you are able to reach the exact same temperatures, voltages and currents inside the SEM as you can inside the TEM while easily swapping chips between microscopes.

Another important feature of the In Situ TKD Stage is the uniform workflow it offers. Because both the TKD Stage and our In Situ TEM solutions operate with the same stimuli supply components and control software, existing customers can easily integrate the TKD stage into their workflow.

What is the compatibility of the In Situ TKD Stage?

The TKD stage is compatible with different brands of SEM/FIBs, namely JEOL, Thermo Fisher Scientific (FEI) and Zeiss. It is also compatible with EBSD detectors from different companies, namely Bruker and Oxford Instruments. We are also looking into the possibility of expanding the compatibility of the stage to more brands. If you are using a different SEM or EBSD detector than the ones listed above, please do not hesitate to contact us.

Who are the people that will benefit from it?

There are a few types of users who will benefit from the TKD stage. This includes users who are interested in analyzing the grains structure and crystal orientation of samples under in situ heating and/or biasing stimuli. For others, the interest lies in the ability to conduct in situ heating and biasing experiments without so much focus on the orientation maps. For these users, the TKD Stage can be used as a simple in situ SEM stage that is more time and cost effective compared to that of a TEM for performing dynamic experiments.

What kind of challenges were tackled during development?

One of the greatest challenges we faced when developing the In Situ TKD Stage was ensuring the widest compatibility without sacrificing its performance. Moreover, we spent a long time on ensuring the flexibility and user-friendliness of the stage. We wanted the TKD Stage installation to be straightforward and effortless, but also flexible to change the orientation of the chips/samples. We also focused on ensuring that the working would be swiftly reached, and that the Nano-Chip positioning inside the TKD stage would be easy.

Another challenge was making the stage compatible with our Wildfire and Lightning Nano-Chips. We wanted to make sure that this was possible so that our Wildfire and Lightning customers could simply purchase the TKD stage and reuse their existing chips and heating/biasing control hardware and software.

Despite these challenges, we managed to fulfil all critical requirements and more. The stage is exceptionally easy to operate, installation takes no more than 10 minutes (even including replacing a flange for a vacuum electrical feedthrough) and the operating vacuum can be reached immediately after the installation within 10 minutes.

Did we cooperate with customers on this development?

Our policy at DENSsolutions has always and will always be to involve users when developing new products. We believe that it is simply impossible to create exceptional products without customers’ involvement.

Following our approach, we involved Vijay Bhatia from University of Sydney during the development of the In Situ TKD Stage. He informed us of necessary requirements for the stage from an experimental point of view, allowing us to design as optimally as possible.  

Which future developments lie ahead?

We will continue to work on the user-friendliness of the TKD stage and its compatibility. Particularly, we will focus on the implementation of an automatic electrical connection of the TKD stage with the control hardware outside the SEM/FIB. Additionally, we will make it possible to integrate our control software into the EBSD/TKD software. This will allow you to sync the crystallographic and in situ stimuli data, simplify the analysis and even control the in situ TKD stage directly from the SEM/FIB software.

Read more about the TKD Stage

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