Transmission Electron Microscopy

Structural & Morphology Characterization (Electron and ion beam technologies)

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TEM and STEM are related techniques which can be considered as the most powerful tools to characterise nanomaterials and indispensable for nanotechnology. In both cases, high energy electrons, incident on ultra-thin samples, allow for image resolutions that below the Ansgtrom order. The electron beam travels through the specimen and, depending on the density, crystallinity, orientation, etc. of the material present, electrons are scattered differently, giving rise to an image of the specimen with different contrast features according to specimen properties. In the STEM mode, electrons pass through the specimen, but, the electron optics focus the beam into a narrow spot which is scanned over the sample in a raster. The rastering of the beam across the sample makes these microscopes suitable for analysis techniques such as mapping by energy dispersive X-ray (EDX) spectroscopy, electron energy loss spectroscopy (EELS) and annular dark field imaging (ADF). These signals can be obtained simultaneously, allowing direct correlation of image and quantitative data. By using a STEM and a high-angle detector, it is possible to form atomic resolution images where the contrast is directly related to the atomic number.

Traditionally, TEM/STEM have been mainly applied for imaging, diffraction, and chemical analysis of solid materials. For biological samples, cell structure and morphology are commonly determined whilst the localization of antigens or other specific components within cells is readily undertaken using specialised preparative techniques and, when required specific TEM cooling holder. Nowadays, the availability of specimen holders designed to perform in situ experiments including heating, cooling, biasing, liquid or gas atmospheres, etc. have turned the TEM into a real nanolaboratory suitable for an increasing range of specimens both in Materials and Llife Science.

A TEM can also be used to do Electron Tomography, which allows obtaining detailed three dimensional (3D) structural and chemical characterisation of 3D objects. This is accomplished by multiple views of the same specimen obtained by rotating the angle of the sample along an axis perpendicular to the beam. By taking multiple images and/or chemical maps of a single TEM sample at differing angles, its 3D structure and composition can be retrieved.

In the last few years, there has been a considerable revolution in electron microscopy with the arrival of aberration correctors for the condenser and objective lenses with the consequent improvement in the attainable resolution limits. The obtainable resolution limit now lies at around 0.05 nm in both TEM and STEM, and the improved images from these aberration-corrected microscopes are opening up new avenues in the characterisation of materials. The use of aberration correctors allows using lower accelerating voltages while keeping atomic resolution and, in combination with the last generation of direct detection cameras and dose modulators, beam sensitive materials can now be observed in the TEM at very low energy and radiation doses.

Sample preparation is the most crucial part in TEM experiments. High quality TEM specimens have a thickness that is comparable to the mean free path of the electrons that travel through the samples, which may be only a few tens of nanometres. Preparation of TEM specimens is specific to the material under analysis and the desired information to obtain from the specimen. Sample preparation laboratories are equipped with the basic tools (diamond saw, polisher, dimpler, electropolisher, ultrasonic cutter, precision ion polishing system, gentle mill, plasma cleaner) commonly used in conventional chemical and mechanical thinning procedures.

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          provided at NFFA-Europe laboratories by:
CNR-IOM (TS)
Italy
CNR-DSCTM
Italy
CEA/LETI
France
C2N-CNRS
France
CSIC-ICMAB
Spain
ICN2
Spain
INL
Portugal
JRC - ISPRA
Italy
KIT
Germany
LUND + MAX IV
Sweden
UAB
Spain
EURONANOLAB
France
CCiTUB
Spain
CNR-IOM (TS)
Italy
JEOL JEM 2010F UHR TEM/STEM
Transmission Electron Microscopy/Scanning Transmission Electron Microscopy
High-brightness thermally assisted field emission gun (FEG), spherical aberration coefficient of the objective lens: (0.47±0.01) mm
Beam voltage: 80-200 kV
STEM attachment High-angle annular dark field (HAADF) for Z-contrast imaging
≤0.13 nm probe size 0.11 nm phase contrast 0.123 nm HAADF/STEM
Constant temperature with a drift rate < 0.1°C/min, with low noise and minimal turbulence
EDX with ultra-thin window for light elements sensitivity (Z > 5)
CSIC-ICMAB
Spain
TEM - JEOL JEM 1210
Image mode: information about the size, morphology, homogeneity and microstructure of the samples. Diffraction mode: determination of the cell parameters, space group and superstructures, incommensurate modulations
Thermionic emission from a tungsten filament
Accelerating voltage: 120 KV
CCD camera ORIUS 831 SC 600 GATAN, suitable for imaging and electron diffraction registration
Point to point resolution of 3.2 Å
Particulate materials (powders, nanoparticles, nanowires..)
Standard single tilt holder and analytical specimen holder of double tilt (Tilt X=± 60o, Tilt Y=± 30o), GATAN 646 model, that allows exploring large volumes of reciprocal space by electron diffraction
JCNS @MLZ
Germany
TEM JEOL JEM-2200F
Soft Matter investigation by room temperature TEM as well as Cryo-TEM on frozen thin specimen in liquid state and solid thin sections of polymers. Detailed information is available at https://mlz-garching.de/tem Real space investigations performed to extract information about shape, size and size distribution of particles, their self-assembly and aggregation.
Field Emission Gun
200 kV acceleration voltage
Image recording on 2k by 2k CMOS Camera from Tietz Video Imaging and Processing System (TVIPS)
Image resolution around 0.17 nm in theory, but 2 nm for room-temperature TEM and 5 nm for Cryo-TEM due to the actual (temporary) environment
Standard vacuum (10-6 Pa range) inside the instrument column
Specimen preparation devices for soft matter: - Leica EM GP grid plunger for thin film of aqueous and organic solvent solution onto Cryogen (liquefied Ethane) - Leica SCD050 for glow discharge to prepare the grid prior to freeze-plunging - Leica UC-7/FC-7 Cryo-ultramicrotome using glass and diamond knife to perform ca. 100 nm thin cryo-sectioning on bulk polymer or resin embedded block specimen. - Leica Freeze Fracture and Etching BAF060 to produce replicas from solution samples.
3 mm holey carbon coated cupper grids. 3 mm standard cupper grids. Gold grids on demand. Thin liquid specimen, thin (ca. 100 nm) sections, eventually sample in powder state
TEM sample can be moved plus/minus 1 mm in X and Y and tilted plus/minus 23° in X direction (Goniometer) 4 positions RT-TEM holder and 2 positions Cryo-TEM holder
ICN2
Spain
TEM – FEI Tecnai G2 F20 HRTEM
High resolution (S)TEM imaging, chemical composition analysis and electron tomography
ZrO2/W (100) Schottky field emission gun
Beam voltages: 80kV, 120kV and 200kV
High resolution transmission electron microscopy (HRTEM) High resolution scanning transmission electron microscopy (HRSTEM) with bright filed (BF), dark filed (DF) and high angle annular dark field (HAADF) modes Energy Dispersive X-ray Spectroscopy (EDX) Electron Energy Loss Spectroscopy (EELS) Energy filtered TEM (EFTEM)
Point resolution: 0.24 nm Information limit: 0.102 nm
High vacuum @ sample level: 10-5Pa
Up to ~100nm thick samples
Automated collection of tilt series (electron tomography) in TEM or STEM mode Inspect 3D and Amira software for tomographic reconstruction
LUND + MAX IV
Sweden
JEOL 3000F TEM
Imaging and analysis at the nano-level via conventional transmission electron microscopy (TEM), high resolution TEM, scanning TEM, and EDXS (energy dispersive Xray spectroscopy)
Field emission gun
300kV accelerating voltage
Image recording on 4k by 2.7k Orius camera from Gatan. EDXS detection on 80mm SSD from Oxford Instruments.
Image resolution around 0.17nm (TEM) and 0.2nm (STEM). Note neither image nor probe is aberration-corrected.
Standard vacuum in the microscope column
Plasma cleaner to remove hydrocarbons that cause contamination in the microscope. Image-processing programs and Image calculation programs available.
3mm standard TEM samples
TEM sample can be moved plus/minus 1mm in X and Y, and tilted plus minus 10 degrees in two axes (double tilt holder)
Spectral resolution 130eV approx. on EDXS
UAB
Spain
TEM JEOL 2011
Conventional transmission electron microscopy (TEM), high resolution TEM, and EDXS (energy dispersive X-ray spectroscopy)
LaB6 filament
Beam Voltage: 200 kV
CMOS Gatan Rio 16. X-Ray detector EDS Oxford Instruments X-max
0.18 nm at 200 kV
3mm standard TEM samples
Ultramicrotomy for polymers and life science samples
Single tilt holder
CIC biomaGUNE
Spain
Multimode V from Bruker
CIC biomaGUNE
Spain
TEM – JEOL JEM-2100F UHR
CIC biomaGUNE
Spain
TEM – JEOL JEM-2100F UHR
EURONANOLAB
France
TEM at EURONANOLAB - CEITEC
EURONANOLAB
France
TEM at EURONANOLAB - IMM
JRC - ISPRA
Italy
Transmission electron microscopy (TEM)
Transmission electron microscopy (TEM) is a microscopy technique able to analyse ultrathin specimens through which an electron beam is transmitted forming an image. This microscope is used to characterise nanomaterials size and morphology and, if combined with energy dispersive x-ray spectroscopy (EDX), elemental composition. TEM is widely used to study cellular ultrastructure and to identify nanomaterials in complex matrices.
UAB
Spain
TEM-JEM 1400
Imaging via conventional transmission electron microscopy (TEM)
Tungsten filament
Accelerating voltage: 120 KV
CCD GATAN Orius camera. CCD REDLAKE MegaPlus II camera.
Point to point resolution of 3.2 Å
3mm standard TEM samples
EURONANOLAB
France
TEM at EURONANOLAB - Nanotec
INL
Portugal
TEM JEM 2100
TEM Imaging, STEM Imaging, Cryo, EDXS
KIT
Germany
TFS Themis Z double corrected
energy materials, electrochemical energy storage, heterogeneous catalysis, quantum materials, nanocrystalline metals, nanocomposites, graphene, multiferroics
S-FEG
60, 80, 300 kV
TEM (BF, DF, HRTEM) with Gatan OneView or K3 camera, STEM (BF, DF, ADF, HAADF, quadrant detector), 4D-STEM (orientation mapping, PDF, DPC, ptychography), EELS (with K3 camera), EDX (Super-X detector)
0.06 nm in TEM and STEM mode at 300 kV
high vacuum, temperature range between LN2 and 1200°C, in-situ heating, electrical, mechanical and gas environment (up to 1 bar)
double corrected, monochromated
0.15 eV
KIT
Germany
TFS Themis 300 probe corrected
energy materials, electrochemical energy storage, heterogeneous catalysis, quantum materials, nanocrystalline metals, nanocomposites, graphene, multiferroics
S-FEG
80, 200, 300 kV
TEM (BF, DF, HRTEM), STEM (BF, DF, ADF, HAADF, segm. STEM detector), 4D-STEM (orientation mapping, PDF, DPC, ptychography) with Dectris Quadro pixelated detector, EDX (Super-X detector)
0.07 nm in STEM mode, 0.19 nm in TEM mode at 300 kV
high vacuum, temperature range between LN2 and 1200°C, in-situ heating, electrical, mechanical and gas environment (up to 1 bar)
probe corrected, precession (NanoMegas ASTAR)
0.7 eV
CCiTUB
Spain
TEM - JEOL ARM200cF, ‘NEOARM’
Materials for energy production and storage, electronics and spintronics, catalysis, 2D materials, multiferroics, metallurgy, photonics, MOFs, biology, macromolecules, etc.
Cold FEG
30, 80, 200 kV
- Cameras: Gatan Rio (CMOS Technology), Gatan K3 (direct detection, post GIF). STEM detectors: BF, ADF, HAADF, ABF, secondary electrons, backscattered electrons. 4D STEM. - Spectroscopies: dual EDXS detectors (2x100mm2, SDD, windowless), GIF Continuum with K3 camera for EELS.
In situ capabilities: Liquid N2 holder, heating + biasing holder, liquid cell holder + heating/biasing.
Electrostatic dose modulator. High tilt analytical tomography holder. Electron beam precession (ASTAR from NanoMegas)
0.26 eV (FWHM ZLP)