SBIR-STTR Award

Continuous Rotation Transmission Electron Microscopy Tomography Stage for Imaging/Spectroscopy and In-Situ Characterization of Materials
Award last edited on: 1/5/2023

Sponsored Program
SBIR
Awarding Agency
DOE
Total Award Amount
$1,350,000
Award Phase
2
Solicitation Topic Code
C49-15c
Principal Investigator
Norman J Salmon

Company Information

Hummingbird Precision Machine (AKA: Hummingbird Scientific)

2610 Willamette Drive NE
Lacey, WA 98516
   (360) 252-2737
   info@hummingbirdscientific.com
   www.hummingbirdpm.com
Location: Single
Congr. District: 10
County: Thurston

Phase I

Contract Number: DE-SC0020543
Start Date: 2/18/2020    Completed: 11/17/2020
Phase I year
2020
Phase I Amount
$200,000
Electron tomography produces high-resolution three-dimensional views of materials. This microscopy technique is poised to have a leading role in structural characterization and development efforts of next generation nano-scale samples of energy materials. The goal and product of electron tomography is to acquire images 2D projections) of the specimen at different angles and reconstruct them into a 3D representation of the sample. For a given processing algorithm, the ultimate quality and spatial resolution of the tomogram depends on the quality and spatial resolution of its parent “tilt series”, the set of acquired 2D raw images at different angles. With the advancement in the aberration corrected TEM high-resolution imaging at low acceleration voltage and direct electron detectors, the high-resolution imaging of nano-scale samples at atomic resolution can be routinely realized. Therefore, the current limitations in the way that tomograms are obtained to construct 3D maps, are found in the lack sample stability. This is due to how the sample is rotated in the TEM as images are acquired; using the built-in TEM stage which was never designed with the requirements in mind needed for these high- resolution 3D tomograms. As a result, the time it takes to acquire image data is very slow. For example, any image shift during rotation requires manual re-alignment of the location and focus of the sample – this all cost time and can add up specifically when small angle steps are taken for highest quality reconstruction. This extra time also results in additional electron dose to the sample. These mechanical limitations hinder advances in the technique, limiting the quality and spatial resolution of tomograms as well as the velocity at which tomograms can be acquired—this latter parameter is paramount for samples that need to be dose-limited during characterization. The main goal of this SBIR project is to build a continuous, ultra-stable, low-vibration, dedicated tomography imaging TEM sample holder and a continuous tomography in-situ biasing TEM sample holder with the purpose of collecting 360 degree tomograms in under 60 seconds. This holder will also specifically use the ability of current generation of high-frame rate TEM cameras to collect data as sufficiently high quality as the sample rotates. We will also develop support hardware to enable FIB sample preparation of samples with an exact concentric center. We will leverage the internal capabilities at Hummingbird Scientific to design, build and test electron microscopy and FIB sample holder systems to develop the hardware in proposed in this project. Materials research groups focused on studying the in-situ and ex-situ 3D structure of nano-scale materials would be the main customer of this product as this hardware can be used in any existing TEM with side-entry stage.

Phase II

Contract Number: DE-SC0020543
Start Date: 4/4/2022    Completed: 4/3/2024
Phase II year
2022
Phase II Amount
$1,150,000
Electron tomography produces high-resolution three-dimensional views of transmission electron microscopy samples. This microscopy technique is poised to have a leading role in future structural characterization efforts of relevant samples in next-generation electronic and energy storage devices that increasingly rely on small complex 3D geometries to push performance to the next level. Only when one can characterize the materials in 3D space can one understand and optimize their performance as well as the processes that are used to fabricate them. At present, the current limiting factor in the speed and quality of transmission electron microscopy (TEM) tomographic reconstructions is the total runout in the tilt axes on modern transmission electron microscopes. As a result, for every tilt step, one must correct for sample shift, which makes tomographic dataset collection a slow and tedious process. The built-in microscope stage (side-entry goniometer) was simply not designed with the specifications needed to produce high- resolution 3D tomograms quickly and repeatably. Slow acquisition also results in unnecessarily high electron doses which can result in damage to the specimen under observation. In Phase I of this SBIR, Hummingbird Scientific has prototyped a fast, concentric moving (low runout) dedicated tomography sample stage that we intend to commercialize as a replacement internal stage product for any TEM. We have successfully demonstrated the advantages of this approach by retrofitting a working transmission electron microscope with our prototype in Phase I. In Phase II, Hummingbird will design, manufacture, assemble, and beta test this internal tomography stage with a tomography sample loading system and control interface for collecting 180-degree tomograms. The final target is to be able to collect a full tomogram in 60 seconds. Our tomography stage product will take full advantage of the current generation of high-frame- rate electron detectors to collect data of sufficiently high quality as the sample rotates. We will leverage the internal capabilities at Hummingbird Scientific to engineer, build, and test this tomography stage system and to develop the commercial product proposed in this project. We have added a second TEM in our facility dedicated for TEM stage work to enable our technicians to perform routine assembly and testing work on TEM columns to support this project. Materials research groups focused on studying the 3D structure of nano-scale materials would be the main customer of this product. We plan to be in beta testing this product and collecting scientifically relevant data to be used in marketing activities by the end of Phase II