|1580 Series||Biasing Transfer||3 mm Sample Transfer|
|High Vacuum Transfer
|Inert Gas Transfer
|Number of Electrical Contacts||9*||0|
|Contact Type||Direct Chip Contact||N/A|
|Settled Resolution||Up to TEM Resolution||Up to TEM Resolution|
|High Temperature On-Chip Sample Heating||Yes||No|
|TEM Compatibility||TFS/FEI, JEOL||TFS/FEI,JEOL|
How It Works
Hummingbird Scientific offers air-free transfer of samples using two TEM platforms with distinct sample geometries:
- MEMS Chip with Biasing Contacts
- Standard 3mm TEM Grid
Both these Air-Free Transfer TEM holders protect your TEM sample from exposure to air between the preparation chamber and the TEM.
Based on the type of the transfer holder (MEMs chip vs. TEM grid), the sample is loaded onto the MEMS biasing chip or the TEM grid of the holder tip inside the preparation chamber (e.g. a glove box) for the transfer. After loading the sample, the tip is retracted into the body of the holder and hermetically sealed in either an inert gas environment or high vacuum. Once inside the TEM, the sample tip is opened to allow TEM imaging and in-situ TEM experiments.Edit
Vacuum/Inert Gas Transfer, Electrical Biasing & Imaging
To perform a successful transfer of an air-sensitive sample from a preparation chamber to the TEM, it is important to consider the best environment to keep the sample free of damage. Some air-sensitive samples transfer best under high vacuum environments, whereas others are best transferred in inert gas conditions.
Hummingbird Scientific’s Air Free TEM Transfer Holders are designed to hold both a positive pressure over the atmosphere for an inert gas transfer (Figure Top Left) or hold a high vacuum during a transfer (Figure Bottom Left).
The holder combines air-free transfer with highly stable imaging capabilities (Figure Top Right – taken with JEOL 2100 200 kV LaB6 TEM).
The holder’s biasing version has up to 9 electrical biasing contacts for on-chip electrical biasing and heating (for example: in-situ TEM data showing current-voltage measurements as a function on time in Figure Bottom Right). The holder’s 3 mm grid version of the holder similarly allows TEM characterization of air-sensitive samples.
Both the transfer holder models are excellent tools for in-situ or standard TEM of air-sensitive solid-state energy storage device materials.Edit
Hummingbird Scientific’s Air-Free Transfer TEM Sample Holders enable the transfer of air-sensitive samples from the preparation chamber to the TEM inside the holder, either in high vacuum or in inert gas conditions. Example applications of this holder are in-situ materials experiments with air sensitive materials for:
- Solid-state electrolyte battery materials
- Nano-scale semiconductor materials
This holder comes in two versions:
- On-chip electrical biasing with 9 pins for in-situ biasing and imaging
- 3mm grid samples for transfer and imaging in the TEM
- Accessories available for your Air-Free Transfer TEM Holder:
- Specialized Heating/Biasing and Biasing MEMS Chips
- MEMS Heating/Biasing Controller
- Specialized Sample Biasing Substrate (e.g., FIB Prep)
- Biasing Power Supplies – Contact Us for Configurations
- Vacuum Tip Cover
Air-free transfer of air-sensitive solid-state battery electrolyte material
Solid-state batteries are generally non-flammable and have been studied for use in future electric vehicles. However, solid electrolytes are known to be highly sensitive to air and moisture. This prevents the utilization of transmission electron microscopy (TEM) to perform high-resolution structural and chemical analysis, as common sample preparation and transfer approaches usually lead to unwanted air exposure. Hummingbird Scientific’s Air-Free Transfer TEM holder allows the air-free transfer of samples from a dry environment (i.e., a glove box) into the TEM.
Researchers at Toyota Research Institute of North America and the University of Pennsylvania successfully transferred air-sensitive solid-state electrolyte material (Lithium Thiophosphate – LPS) inside the TEM for in-situ structural and spectroscopic analyses. There are clear differences between samples transferred with and without the TEM transfer holder (Figure – Right). The LPS particle transferred using the Air-Free Transfer TEM holder shows no sign of surface oxidation and degradation. The electron dispersive spectroscopy (EDS) data confirms no significant level of oxygen on the surface. The same LPS material transferred to the TEM in a standard holder without a protective mechanism (Figure – Bottom Right) undergoes surface oxidation resulting in a porous microstructure.
Data Courtesy: Dr. Nikhilendra (Nik) Singh and Dr. Timothy S. Arthur, Toyota Research Institute of North America, James Horwath and Dr. Eric Stach, University of Pennsylvania.Edit