|Tilt Range||Up to ± 45° depending on objective pole||Up to ± 20° (alpha and beta) depending on objective pole|
|Beta-tilt accuracy||NA||<0.01 degree|
|Contact Type||Direct Chip Contact||Direct Chip Contact|
|Max Operating Temperature||> 1000°C||> 1000°C|
|Settled Resolution at 1000°C||Up to TEM resolution||Up to TEM resolution|
|Temperature Stability||+ 100 hours||+ 100 hours|
|Temperature Measurement||4-point resistance sensing||4-point resistance sensing|
|EELS / EDS Compatible||Yes (full temp range)||Yes (full temp range)|
|TEM Compatibility||TFS/FEI, JEOL, Hitachi||TFS/FEI, JEOL, Hitachi|
Hummingbird Scientific’s in-situ TEM MEMS Biasing/Heating Sample Holder allows users to heat and/or electrically bias their sample inside the TEM. Heating can be performed to > 1000°C in closed loop control with an on-chip sensor.
The system features:
- Direct chip contact insertion mechanism—no fragile probes that make inconsistent contact involved, so easy to use.
- Standard MEMS chip biasing/heating with 9 contacts
- Single and double tilt configurations
- 4-point temperature sensing method
- Shielded electrical cables for low current measurements
- Integrated heating and voltage source meter controller
- Intuitive graphical user interface for system control
- EDS compatible over the full temperature range
The system is available as a single-tilt and double-tilt version. The double-tilt holder features a high-accuracy (<0.01 degree) beta-tilt mechanism and no tilt-backlash when changing tilt direction, making it the most stable and usable double-tilt holder available.Edit
Accurate and repeatable beta-tilt
Accurate and repeatable beta-tilt
The beta-tilting resolution and accuracy of this double-tilt Heating + Biasing TEM holder are <0.01 degree. The negligible backlash one gets when reversing tilt direction that often makes other double-tilt TEM holders difficult to use is in the same order of magnitude.
The figure on the left shows beta-tilt from 0 to 0.3 to 0 degree with an exact return to 0.0 after tilting the same amount of steps in both directions.Edit
Hummingbird Scientific’s Heating + Biasing TEM holder platform is supported by our microfabrication team. All our MEMS chips are designed, fabricated, and tested in-house to assure optimal performance and quality.
Our fabricated MEMS chips-based microheaters provide:
- Temperatures > 1000°C
- 4-point resistance sensing
- > 100 hours of temperature stability
- Large field of view
- Compatibility with electron-based spectroscopy (EELS and EDS)
Learn more about our microfabrication facilities here.
Hummingbird’s Scientific Heating + Biasing sample holder has an industry leading 9 contacts (standard). All electrical contacts are available for non-heating biasing experiments with our biasing MEMS chips. While using the heating + biasing capability with our Heating-Biasing MEMS chips, four contacts are used for heating and sensing; the remaining five contacts are available for biasing the sample.
Hummingbird Scientific’s graphical user interface features intuitive controls for heating and biasing functions, including temperature-set point and voltage sweeps. Custom camera integration options are available.
All our MEMS chips are designed, fabricated, and tested in-house, and are available in our web store for our customers.Edit
Segregation of 2D MoS2 Layers into quantum dots during in-situ high temperature heating
Few-layer 2D MoS2 samples were transferred onto the open viewing area of the MEMS heating chip (Figure (a) ) layered with residual organic layers from the transfer process. Heating up the MoS2 sample to 1000°C resulted into a 2D material with well segregated MoSx quantum dot particles embedded in carbon based-composites and areas with pure MoS2 (Figures (b)-(d) ). Particles smaller than 10 nm were observed and many display hexagonal crystal facets. The segregation happens at temperatures >1000 °C. Energy-dispersive X-ray spectroscopy (EDS) confirmed the chemical content of each segregated area. The example shows a dark-field STEM image at a temperature of 1000 °C, together with the EDS map proving the elemental segregation.
Data provided by Jay Horwath, Deep Jariwala and Eric Stach from the University of Pennsylvania.
Figure (a) BFTEM image of as-transferred 2D MoS2 flake on heater chip; (b) DFSTEM Sample heated to 1000°C showing segregation after melting events; (c) DFSTEM image showing MoSx quantum dots (light particles) embedded in carbon-rich region (dark matrix) and un transformed MoS2 (grey regions); (d) elemental EDS mapsEdit
Customization & Service
|Alexander B. Bard, Matthew B. Lim, Xuezhe Zhou, Julio A. Rodriguez Manzo, Daan Hein Alsem, and Peter J. Pauzauskie. “Observation of Void Formation in Cubic NaYF4 Nanocrystals Using In Situ Heating Transmission Electron Microscopy,” Microscopy & Microanalysis (2019)||Abstract|
|Khim Karki, Victoriea L. Bird, Daan Hein Alsem, and Melissa K. Santala. “In Situ TEM Observation of Crystallization in Phase-Change Material,” Microscopy & Microanalysis (2018)||Abstract|
|Victoriea L. Bird, Al J. Rise, Khim Karki, Daan Hein Alsem, Geoffrey H. Campbell, and Melissa K. Santala. “Mapping Crystallization Kinetics of Phase-Change Materials Over Large Temperature Ranges Using Complementary In Situ Microscopy Techniques,” Microscopy & Microanalysis (2018)||Abstract|
|Daan Hein Alsem, James Horwath, Julio Rodriguez-Manzo, Khim Karki and Eric Stach. “Optimized High-Temperature In-Situ Transmission Electron Microscopy Double-Tilt Sample Heating Platform,” Microscopy & Microanalysis (2019)|
|Daan Hein Alsem, James Horwath, Julio Rodriguez-Manzo, Khim Karki and Eric Stach. “In-Situ Transmission Electron Microscopy Double-Tilt Sample Heating Platform.” Microscience Microscopy Congress (2019)|
|Khim Karki, Victoriea L. Bird, Julio Rodriguez-Manzo, Daan Hein Alsem, Norman Salmon, and Melissa K. Santala. “Direct Observation of Crystallization in Phase-Change Material Using In-Situ TEM,” International Microscopy Congress (2019)|
|Victoriea L. Bird, Al J. Rise, Khim Karki, Daan Hein Alsem, Geoffrey H. Campbell, and Melissa K. Santala. “Measuring Crystal Growth Rates in an Amorphous Ag-In-Sb-Te Phase-Change Material Over Large Temperature Ranges Using In-Situ Microscopy Techniques,” Materials Science and Technology (2018)|
|Xuezhe Zhou, Julio Alejandro Rodriguez Manzo, Matthew Lim, Norman Salmon, and Peter Pauzauskie. “Tracking Thermal Phase Transformations of Luminescence Materials with In-Situ TEM” Materials Research Society (2017)|