Research Group Prof. Christian Kübel

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The electron microscopy and spectroscopy group is operating the following equipment at the Institute of Nanotechnology (INT) in Karlsruhe, which is available for research activities within HIU:

Laboratories

• SEM, FIB and TEM laboratories
• Metallography laboratory for SEM/TEM sample preparation
• Sample preparation laboratory for battery materials with MBRAUN glovebox equipped with micromanipulator controlled sample handling
• Image processing laboratory with specialized software for SEM and TEM image analysis and processing

Equipment

Transmission Electron Microscopes (TEM)

Transmission electron microscopy (TEM) enables characterization of materials by direct imaging with up to atomic resolution. The image information can be locally correlated with spectroscopic techniques (EELS/EFTEM and EDX) to provide semi-quantitative elemental composition/maps with sub-nanometer resolution. All of these techniques can also be performed in-situ, e.g. during heating, electrical biasing or straining to directly correlate structural changes and materials properties. Furthermore, for complex three-dimensional structures, electron tomography can be used to generate a 3D representation of the material with a spatial resolution of 1–2 nm.

FEI Titan 80-300 Transmission Electron Microscope

• FEG
• Image aberration corrector
• Gatan Ultrascan US1000 CCD camera
• HAADF-STEM detector
• Gatan GIF 863
• EDAX S-UTW EDX detector
• Resolution: 0.08 nm information limit TEM, 0.14 nm resolution in STEM, 0.7 eV energy resolution EELS
• Imaging and Analysis Techniques: BF-TEM, aber. cor. HRTEM, HAADF-STEM, HRSTEM, EFTEM, EELS, EDX, (S)TEM tomography, Electron diffraction, Lorentz imaging, Low-dose techniques & cryo imaging

FEI Titan 80-300 Transmission Electron Microscope

• FEG
• Gatan Orion CCD camera
• HAADF-STEM detector
• Gatan GIF2001
• EDAX S-UTW EDX detector
• NanoMegas ASTAR System with TopSpin
• Resolution: 0.15 nm information limit TEM, 0.19 nm resolution in STEM, 0.7 eV energy resolution EELS,
• Imaging and Analysis Techniques: BF-TEM, aber. cor. HRTEM, HAADF-STEM, HRSTEM, EFTEM, EELS, EDX, (S)TEM tomography, (Precession) Electron diffraction, Low-dose techniques & cryo imaging, Orientation mapping

TEM holders for both TEMs

• Analytical single-tilt holder
• Analytical double-tilt holder
• Tomography holder – Fischione 2020
• Double-tilt heating holders: Protochips Aduro 300: RT-1200ºC (MEMS based), Gatan 652: RT-800ºC (classical holder)
• Cryo-holder: Gatan 915: LN2-80ºC
• Straining holders: Hysitron Picoindenter PI95 with nanoindentation and straining with PTP, Gatan 654 heating straining holder
• Electrical Biasing – Protochips Aduro 300
• Electro chemistry – Protochips Poseidon 510

Focused Ion Beam (FIB) Systems

The FEI Strata 400S and the Zeiss Auriga 60 Dual Beam FIB are both a combination of a scanning electron microscope (SEM) and a focused ion beam (FIB) system, which allows imaging and structuring of materials at the nanoscale. The focused gallium ion beam can either be used for ion imaging or to cut predefined patterns or images in the surface of a solid. At the same time, the SEM can be used to image the nanostructures generated by FIB. In addition, it is possible to locally deposit C, Pt or W from precursor gases using the electron or ion beam. Using this combined approach it is possible to

• perform cross-sectional structural analysis of surfaces
• extend the cross-sectional analysis by slice and view techniques to image a complete 3D volume
• pattern surface at the nanoscale
• electrically contact selected structures on a sample
• target preparation of TEM samples and in-situ lift-out

Zeiss Auriga 60 FIB

• Electron Optics: 1.0 nm resolution at 15 kV, 1.9 nm resolution at 1 kV, Operation voltage: 200V -30kV
• Gallium Ion optics: 2.5 nm resolution at 30kV, Operation voltage: 200V – 30kV
• FEG electron source
• In-lens SE, ETD, EsB, 4QBSD, SESI detectors for SEM imaging
• STEM detector
• EDAX EBSD+EDX detector
• Omniprobe 400
• GIS for C, Pt, W, Si
• Gas injection charge compensation

FEI Strata 400 S DualBeam FIB

• Electron Optics: 1.0 nm resolution at 15 kV, 1.9 nm resolution at 1 kV, Operation voltage: 200V -30kV
• Gallium Ion optics: 7 nm resolution at 30kV, Operation voltage: 2-30kV
• FEG electron source
• TLD SE, ETD, BSE, CDEM detectors for SEM imaging
• STEM detector
• EDAX EDX detector
• Omniprobe 100
• GIS for C, Pt, and W
• GIS for XeF₂ etch enhance
• Flip-stage

• Sample Preparation
• Fischinione NanoMill 1040 for site selected low-voltage argon ion thinning of TEM samples
• Gatan 691 Procission Ion Polishing Systems equipped with low-voltage option and optional cryo cooling
• Struers TenuPol-5 electropolishing system
• Cressington 328 high-vacuum carbon/metal sputter coater, Cressington 108 carbon coater
• Fischione 1020 Plasma Cleaner
• MBRAUN glovebox with homebuild SmarAct micromanipulator system
• Various optiocal microscopes (Leica AxioTech, Leica S6E, Leica M80, Keyence VHX-500)
• Bulk sample preparation (Sommer GS-1000 wire saw, Gatan 656 dimple grinder, Gatan 623 disc grinder, Struers RotoPol-21 polisher, Struers RotoPol-25 polisher, Struers LaboPress-1 infiltration system)