LabAdviser/314/Microscopy 314-307/TEM/ETEM

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This section is written by DTU Nanolab internal if nothing else is stated.

Titan ETEM in building 314.

FEI Titan 80-300 ETEM

The Titan ETEM is a transmission electron microscopy equipped with a field emission electron source (FEI X-FEG), a monochromator and an aberration corrector on the super-twin (S-TWIN) objective lens (CEOS CESCOR). This gives the microscope a resolution of about 0.8 Å in TEM mode. Other tecniques available on the microscope are scanning transmission electron microscopy (STEM, resolution 1.4 Å) with both high-angle annular dark-field (HAADF) and dark-field (DF)/bright-field (BF) detectors. On the analytical side, the microscope is equipped with Oxford X-Max 80T SDD X-ray detector for energy dispersive X-ray (EDS) spectroscopy and Gatan Tridiem 866 imaging filter allowing for electron energy-loss spectroscopy (EELS) and energy-filtered imaging (EF-TEM). For imaging, the microscope is equipped with Gatan US1000 cameras (2048x2048 px) before and after the energy filter, as well as a Gatan OneView camera for fast in situ acquisition (25fps full resolution 4k x 4k, 100fps 2k x 2k, 200fps 1k x 1k, 300fps 512 x 512).

The microscope is equipped with a differential pumping system which allows gases to be introduced around the sample to a pressure on the order of 10 mbar (gas specie dependent). Several gases are permanently mounted on the system: Hydrogen, helium, methane carbon monoxide, nitrogen and oxygen. Additional gases and gas mixtures can be added as needed. Please contact Cen staff if you need other gases.

Schematic of the Titan ETEM differential pumping system.

As a high-resolution TEM, the Titan ETEM is very versatile. It has been used to study materials such as catalysts, steels, graphene, polymers, oxides and fuel cells. The high tension can be varied between 80kV, 200kV and 300kV. If you have special requests, please come and see us.

Sample holders

All TEM sample holders available at DTU Nanolab building 314/307 are compatible with the Titan ETEM. The lab has holders for heating (furnace and MEMS-based), cooling, biasing and tomography. For information on the holder see HERE.

Who may operate the Titan ETEM

In order to start training on the Titan ETEM you must by fully trained in the Tecnai TEM. Most of the basic operation on the Titan ETEM is the same as on the Tecnai with the added complexity of the aberration corrector and the monochromator.

The training is conducted in two steps (as needed). In the first step, you will be trained on the special aspects of the microscope, i.e. the monochromator and the aberration corrector. In the second step, we will familiarize you with the differential pumping system and the gas inlet system.

When you have demonstrated a high level of familiarity with the microscope you are allowed to book it via LabManager and use it 24/7.

Booking

Booking on the ETEM is done by the users in accordance to the booking rules. Booking rules can be found in LabManager under "Documents" for the ETEM. It is important to follow the procedures described in the ETEM Userguide to ensure a clean system for each user and to minimize cross-contamination between experiments.

Further information

Titan ETEM in LabManager

Calibration

• GIF collection angles (20220209)
• Magnification calibration cameras
• Convergence angles STEM

Process information

The following techniques and processes are available on the microscope (list isn't complete):

Techniques:

• EDS/WDS
• EELS
• EFTEM
• Holography

Processes:

• Oxidation/Reduction of metal particles

Tips and Tricks

Here you can find some help to solve small issues on the microscope. Let us know, if you have other suggestions.

• Magic Switch is not working properly
• Description OneView camera
• Aztec connection problems
• GIF apertures are not responding
• HAADF detector doesn't give a signal
• No buttons for STEM acquisition

Selected publications from ETEM groups around the globe

T. W. Hansen et al., Atomic-resolution in situ transmission electron microscopy of a promoter of a heterogeneous catalyst. Science 294, 1508-1510 (2001).

P. L. Hansen et al., Atom-Resolved Imaging of Dynamic Shape Changes in Supported Copper Nanocrystals. Science 295, 2053-2055 (2002).

J. B. Wagner et al., In Situ Electron Energy Loss Spectroscopy Studies of Gas-Dependent Metal-Support Interactions in Cu/ZnO Catalysts. J. Phys. Chem. B 107, 7753-7758 (2003).

S. Helveg et al., Atomic-scale imaging of carbon nanofibre growth. Nature 427, 426-429 (2004).

T. W. Hansen, J. B. Wagner, R. E. Dunin-Borkowski, Aberration corrected and monochromated environmental transmission electron microscopy: challenges and prospects for materials science. Mater. Sci. Technol. 26, 1338-1344 (2010).

T. J. Booth et al., Discrete Dynamics of Nanoparticle Channelling in Suspended Graphene. Nano Lett. 11, 2689-2692 (2011).

T. W. Hansen, J. B. Wagner, Environmental Transmission Electron Microscopy in an Aberration-Corrected Environment. Microsc. Microanal. 18, 684-690 (2012).

W. F. van Dorp et al., Molecule-by-Molecule Writing Using a Focused Electron Beam. ACS Nano 6, 10076-10081 (2012).

H. Yoshida et al., Visualizing Gas Molecules Interacting with Supported Nanoparticulate Catalysts at Reaction Conditions. Science 335, 317-319 (2012).

T. W. Hansen, A. T. Delariva, S. R. Challa, A. K. Datye, Sintering of Catalytic Nanoparticles: Particle Migration or Ostwald Ripening? Acc. Chem. Res. 46, 1720-1730 (2013).

B. K. Miller, P. A. Crozier, Analysis of catalytic gas products using electron energy-loss spectroscopy and residual gas analysis for operando transmission electron microscopy. Microsc. Microanal. 20, 815-824 (2014).

P. A. Crozier, T. W. Hansen, In situ and operando transmission electron microscopy of catalytic materials. MRS Bull. 40, 38-45 (2015).