Every microscope at NCEM is equipped with a single tilt and double tilt holder. In addition to these holders, several other in-situ experiments are possible with the use of the following holders:
ThermoFisher/FEI Microscopes
1. FEI Double Tilt low background holder for FEI
Description: There are four of these holders – one at ThemIS, TitanX, TEAM I and Tecnai. These utilize a three-pronged clip to hold the TEM sample. These are the best holders for the SuperX EDS detectors because of the line-of-sight to the detector. Clips are either Cu or Mo and washers are Cu, Al, or Mo.
Ideal use case: EDS of conventional TEM grids, SiN membranes, FIB liftout on posts, 3mm electropolished or wedge polished.
Compatible TEMs: TitanX, ThemIS, TEAM I, Tecnai
2. FEI Double Tilt low background holder for FEI with hex ring
Description: This holder uses a hex ring to secure the sample and is well-suited for magnetic samples.
Ideal use case: EDS signal is somewhat compromised.
Compatible TEMs: TitanX, ThemIS, TEAM I
3. FEI Single Tilt
Description: There are several single tilt holders for general use. The ones with the Cu cup are preferred over the Be cup for liquid samples. The EDS signal is compromised.
Compatible TEMs: TitanX, ThemIS, TEAM I
4. Gatan 698 Elsa cryo-transfer tomography holder for FEI
Description: The Gatan 698 cryo-transfer tomography holder is a liquid nitrogen based holder
with a thin profile that is compatible with Super-Twin and Ultra-Twin pole pieces. The
temperature can be controlled within a range of -180 to +100 °C using an external controller.
Sample tilt range is +/- 79 degrees in alpha, no tilt in beta. There is a transfer stage to do a cryo-
transfer process. Samples are placed in between two grippers and consequently the holder will
only accept standard grids of ~50um thickness – no SiN membranes. The sample drift is less
than 1.5nm/minute. Prior to using, ensure that the holder dewar has been properly baked.
Ideal use case: The setup is ideal for MicroEDs or Cryo-Tomography. It can also be used to
study phase transitions at low temperature, which may be observed via bright field TEM, or via
electron diffraction. Often, damage in beam sensitive materials is mitigated by the use of a
cooling holder.
Compatible TEMs: TitanX, ThemIS, TEAM I, TEAM 0.5, Tecnai
5. Gatan 915 cryo-transfer holder
Description: The Gatan 915 double cooling holder is a Liquid Nitrogen based holder with a retractable sealing blade, which can enable air-free sample transfer for air-sensitive materials. The temperature can be set within a range of -170 to -100 °C using an external controller. Sample tilt range is limited to +/- 20 degrees in a and +/- 10 degrees on the b axis. Samples are fixed to the holder using a Beryllium hexring, and the holder can accommodate any TEM sample on a 3 mm grid. Similar to the furnace style heating holders, the entire sample is heated all at once. This makes the holder versatile, and capable of handling most conventional TEM samples. However, sample drift is significantly larger in such holders, and precise, hysteresis-free temperature control is not possible
Ideal use case:. The setup is ideal for studying phase transitions at low temperature, which may be observed via bright field TEM, or via electron diffraction. Often, damage in beam sensitive materials is mitigated by the use of a cooling holder. The air free holder is particularly useful when studying air-sensitive samples such as Lithiated compounds.
Compatible TEMs: TitanX, ThemIS, TEAM I
6. Gatan 636 cryo holder for FEI
Description: The Gatan 636 double cooling holder is a Liquid Nitrogen based holder. The temperature can be set within a range of -170 to -100 °C using an external controller. Sample tilt range is limited to +/- 20 degrees in a and +/- 10 degrees on the b axis. Samples are fixed to the holder using a Beryllium hexring, and the holder can accommodate any TEM sample on a 3mm grid. Similar to the furnace style heating holders, the entire sample is heated all at once. This makes the holder versatile, and capable of handling most conventional TEM samples. However, sample drift is significantly larger in such holders, and precise, hysteresis-free temperature control is not possible.
Ideal use case: The setup is ideal for studying phase transitions at low temperature, which may be observed via bright field TEM, or via electron diffraction. Often, damage in beam sensitive materials is mitigated by the use of a cooling holder.
Compatible TEMs: TitanX, ThemIS, TEAM I
7. Gatan 671 Cryo-Straining holder for FEI
Description: The Gatan 671 cryo-straining holder is a single tilt holder. A rectangular opening at the specimen holder tip has two points for securing the specimen; a fixed mounting point at one end and a moveable crosshead at the opposite end. The screw mechanism firmly and securely holds each end of the specimen in place during elongation. A motion controller system is used to apply a constant elongation rate in the range of 2.0 μm/second. A dog-bone sample configuration is preferred, but is not necessary.
Ideal use case: This holder is the easiest way to do an in-situ tensile test in the electron microscope at low temperatures. The variable temperature facilitates tensile tests below the glass transition temperature. The holder can accommodate most TEM samples on a 3mm grid. Strain evolution can be studied via bright field imaging, or electron diffraction, as well as the effect of lattice defects. However, the applied strain is not localized to a specific field of view.
Compatible TEMs: TitanX, ThemIS, TEAM I
8. Gatan 654 Straining holder for FEI
Description: The Gatan 654 straining holder is a single tilt holder. A rectangular opening at the specimen holder tip has two points for securing the specimen; a fixed mounting point at one end and a moveable crosshead at the opposite end. The screw mechanism firmly and securely holds each end of the specimen in place during elongation. A motion controller system is used to apply a constant elongation rate in the range of 2.0 μm/second. A dog-bone sample configuration is preferred, but is not necessary.
Ideal use case: This holder is the easiest way to do an in-situ tensile test in the electron microscope. The holder can accommodate most TEM samples on a 3mm grid. Strain evolution can be studied via bright field imaging, or electron diffraction, as well as the effect of lattice defects. However, the applied strain is not localized to a specific field of view.
Compatible TEMs: TitanX, ThemIS, TEAM I
9. Hysitron picoindentation PI95 holder for FEI
Description: The PI95 picoindentation holder is capable of mechanical deformation experiments in the TEM. The indentation tip is a conical diamond tip, with a front face of ~ 5 mm in size. The holder is a single tilt holder, and samples must be mounted on consumable stubs, which can be purchased from the manufacturer. The holder is equipped with a force transducer, capable of modulating the force on the sample down to ~ 2 µN, and a piezo tube capable of measuring the resulting sample displacement. Using custom stubs, tensile tests are also possible on this holder. Similarly, samples prepared in a notched, bending nano-beam geometry can be used to study fracture in materials. Nanoparticles can be dropcast on silicon wedge mounts (sold by Hysitron as a consumable), and can be studied under compression.
The ECR holder is capable combining electrical contact resistance measurements with nano-indentation. A conducting nano-indentation probe is used, which can be used both for mechanical indentation, as well as current injection. The stress and strain applied on the sample can be recorded using a electrostatic transducer, and a piezo displacement sensor, similar to the PI95 holder. The electrical source meter has a mV and pA resolution in voltage and current.
Ideal use case: While this holder is very versatile, sample compatibility issues can make some experiments very challenging. Typical uses of this holder include studying dislocation migration and as changes in sample morphology under applied mechanical pressure. Phase transitions can be studied via electron diffraction.
Samples can be studied under compression, or tensile stress. However, tensile stress requires the use of E-push to pull chips, and sample preparation often limits the ways in which this holder can be used. As with the PI95 holder, the samples may be imaged in bright field / dark field TEM, or via electron diffraction. It makes sense to study materials where the atomic structure or electronic structure can be tuned under strain. While the atomic structure can be studied through imaging / diffraction, the band structure changes are reflected in the I/V transport curves.
Compatible TEMs: TitanX, ThemIS, TEAM I
10. Gatan 652 heating holder for FEI
Description: The Gatan 652 double tilt heating holder is a furnace style heating holder, capable of heating samples up to 1000 °C. Sample tilt range is limited to +/- 20 degrees in a and +/- 10 degrees on the b axis. Samples are fixed to the holder using a Tantalum hexring, and the holder can accommodate any TEM sample on a 3 mm grid. There are two of these holders; the double tilt feature does not work on the older model.
Ideal use case: Being a furnace style holder, the entire sample is heated all at once. This makes the holder versatile, and capable of handling most conventional TEM samples. However, sample drift is significantly larger in such holders, and precise, hysteresis-free temperature control is not possible. The setup is ideal for studying phase transitions at high temperature, which may be observed via bright field TEM, or via electron diffraction. High resolution imaging is limited by sample drift.
Compatible TEMs: TitanX, ThemIS, TEAM I
11. Protochips Fusion DT biasing/heating holder for FEI
Description: This holder is the newer Fusion model which is compatible with the Axon software. The protochips double tilt biasing/heating holder is equipped with four electrical feedthroughs. The holder can be tilted with a range of +/- 15 degrees in a and +/- 8 degrees in b. Samples are mounted onto e-chips, which should be purchased from Protochips. These e-chips can be made in a variety of configurations to enable both biasing and heating experiments. In the case of heating, the chips include MEMS based heating stages, which localize the heat to a small window, thereby reducing sample drift, and improving holder stability. This also leads to better control over the sample temperature as compared to the Gatan furnace style holders. However, sample preparation is limited by the configuration of the e-chips chosen for the experiment. The holder is equipped with a Keithley 2612 source measurement unit, which is a mV/pA SMU.
Ideal Use Case: This holder is ideally suited for heating and biasing of samples which may be transferred onto e-chips. Since the e-chips include a thin Silicon Nitride membrane, they are quite fragile, and the sample preparation methods are limited to dropcasting, viscoelastic transfers, or FIB liftouts.
Compatible TEMs: TitanX, ThemIS, TEAM I
12. Protochips Aduro DT biasing/heating holder for FEI
Description: This holder is an older model but still compatible with new Protochips MEMs devices. The protochips double tilt biasing/heating holder is equipped with four electrical feedthroughs. The holder can be tilted with a range of +/- 15 degrees in a and +/- 8 degrees in b. Samples are mounted onto e-chips, which should be purchased from Protochips. These e-chips can be made in a variety of configurations to enable both biasing and heating experiments. In the case of heating, the chips include MEMS based heating stages, which localize the heat to a small window, thereby reducing sample drift, and improving holder stability. This also leads to better control over the sample temperature as compared to the Gatan furnace style holders. However, sample preparation is limited by the configuration of the e-chips chosen for the experiment. The holder is equipped with a Keithley 2612 source measurement unit, which is a mV/pA SMU.
Ideal Use Case: This holder is ideally suited for heating and biasing of samples which may be transferred onto e-chips. Since the e-chips include a thin Silicon Nitride membrane, they are quite fragile, and the sample preparation methods are limited to dropcasting, viscoelastic transfers, or FIB liftouts.
Compatible TEMs: TitanX, ThemIS, TEAM I
13. Protochips Aduro ST biasing/heating holder for FEI
Description: This is the older single tilt Aduro model which is still compatible with new Fusion chips. The lower profile makes it compatible with the ultra-twin lens on the Tecnai. The protochips double tilt biasing/heating holder is equipped with four electrical feedthroughs. The holder can be tilted with a range of +/- 15 degrees in a and +/- 8 degrees in b. Samples are mounted onto e-chips, which should be purchased from Protochips. These e-chips can be made in a variety of configurations to enable both biasing and heating experiments. In the case of heating, the chips include MEMS based heating stages, which localize the heat to a small window, thereby reducing sample drift, and improving holder stability. This also leads to better control over the sample temperature as compared to the Gatan furnace style holders. However, sample preparation is limited by the configuration of the e-chips chosen for the experiment. The holder is equipped with a Keithley 2612 source measurement unit, which is a mV/pA SMU.
Ideal Use Case: This holder is ideally suited for heating and biasing of samples which may be transferred onto e-chips. Since the e-chips include a thin Silicon Nitride membrane, they are quite fragile, and the sample preparation methods are limited to dropcasting, viscoelastic transfers, or FIB liftouts.
Compatible TEMs: TitanX, ThemIS, TEAM I, Tecnai
14. Hummingbird biasing holder for FEI
Description: The Hummingbird single tilt biasing holder is equipped with six electrical feedthroughs, which enable in-situ electrical biasing experiments. The feedthroughs terminate in BNC connectors, which can be adapted to most electrical connectors. No specific electronic amplifier is provided with this holder, but typically, a keithley source/measurement unit can be used to provide simultaneous current/voltage readout. Samples are mounted onto PCB boards with glue, and the final electrical connection to the sample must be made via wire bonding or silver paint. The holder does not include cutouts for high signal to noise EDS mapping, but this issue can be overcome by tilting the holder.
Ideal Use Case: This holder can be used to study materials which reconfigure under applied electric fields, such as polar oxides. Similarly, conducting materials can be joule heated, and studied via imaging or diffraction.
Compatible TEMs: TitanX, ThemIS, TEAM I
15. Gatan 648 Double Tilt air free holder
Description: The Gatan air free holder can enable electron microscopy of air-sensitive TEM samples. Sample tilt range is limited to +/- 20 degrees in a and +/- 10 degrees on the b axis. The samples can be loaded on the holder using the hexring mechanism in a moisture-free environment such as the glove box at NCEM. The holder has cutouts for high signal EDS mapping and a retractable tip with a sealing o-ring, which preserves the sample in a moisture free environment. Any sample on a 3 mm grid can be accommodated by the holder.
Ideal use case:. The holder is suitable for studying air-sensitive samples such as Lithiated compounds.
Compatible TEMs: TitanX, ThemIS, TEAM I
16. Fischione Single Tilt air free holder
Description: The Gatan air free holder can enable electron microscopy of air-sensitive TEM samples. Sample tilt range is limited to +/- 20 degrees on the a axis. The samples can be loaded on the holder using a hinged clamp mechanism in a moisture-free environment such as the glove box at NCEM. The holder has cutouts for high signal EDS mapping and a retractable tip with a sealing o-ring, which preserves the sample in a moisture-free environment. Any sample on a 3 mm grid can be accommodated by the holder.
Ideal use case:. The holder is suitable for studying air-sensitive samples such as Lithiated compounds.
Compatible TEMs: TitanX, ThemIS, TEAM I
17. Protochips Poseidon Liquid flow holder for FEI
Description: This holder is available for long-term projects on the ThemIS TEM by special permission. It enables liquid flow using the commercial flow cells available from Protochips.
Compatible TEMs: ThemIS
18. Hummingbird Gas Flow holder for FEI
Description: This holder is available for long-term projects on the ThemIS TEM by special permission. It enables gas flow using the commercial flow cells available from Hummingbird. The temperature can be independently controlled from 20C to 1000C. The holder is compatible with STXM beamline at the ALS for correlative gas flow experiments using x-rays or electrons and generally resides at the ALS.
Compatible TEMs: ThemIS
JEOL Microscopes
19. Gatan 652 heating holder for JEOL
Description: The Gatan 652 double tilt heating holder is a furnace style heating holder, capable of heating samples up to 1000 °C. Sample tilt range is limited to +/- 15 degrees in a and +/- 10 degrees on the b axis. Samples are fixed to the holder using a Tantalum hexring, and the holder can accommodate any TEM sample on a 3 mm grid.
Ideal use case: Being a furnace style holder, the entire sample is heated all at once. This makes the holder versatile, and capable of handling most conventional TEM samples. However, sample drift is significantly larger in such holders, and precise, hysteresis-free temperature control is not possible. The setup is ideal for studying phase transitions at high temperature, which may be observed via bright field TEM, or via electron diffraction. High resolution imaging is limited by sample drift.
Compatible TEMs: JEOL 3010
20. Gatan 654 Straining holder for JEOL
Description: The Gatan 654 straining holder is a single tilt holder. A rectangular opening at the specimen holder tip has two points for securing the specimen; a fixed mounting point at one end and a moveable crosshead at the opposite end. The hexring based clamping mechanism firmly and securely holds each end of the specimen in place during elongation. A motion controller system is used to apply a constant elongation rate in the range of 2.0 μm/second.
Ideal use case: This holder is the easiest way to do an in-situ tensile test in the electron microscope. The holder can accommodate most TEM samples on a 3mm grid. Strain evolution can be studied via bright field imaging, or electron diffraction, as well as the effect of lattice defects. However, the applied strain is not localized to a specific field of view.
Compatible TEMs: JEOL 3010
21. Hysitron picoindentation PI95 holder for JEOL
Description: The PI95 picoindentation holder is capable of mechanical deformation experiments in the TEM. The indentation tip is a conical diamond tip, with a front face of ~ 5 mm in size. The holder is a single tilt holder, and samples must be mounted on consumable stubs, which can be purchased from the manufacturer. The holder equipped with a force transducer, capable of modulating the force on the sample down to ~ 2 µN, and a piezo tube capable of measuring the resulting sample displacement. Using custom stubs, tensile tests are also possible on this holder. Similarly, samples prepared in a notched, bending nano-beam geometry can be used to study fracture in materials. Nanoparticles can be dropcast on silicon wedge mounts (sold by Hysitron as a consumable), and can be studied under compression.
Ideal use case: While this holder is very versatile, sample compatibility issues can make some experiments very challenging. Typical uses of this holder include studying dislocation migration and as changes in sample morphology under applied mechanical pressure. Phase transitions can be studied via electron diffraction.
Compatible TEMs: JEOL 3010
22. Hysitron ECR holder for JEOL
Description: The ECR holder is capable combining electrical contact resistance measurements with nano-indentation. A conducting nano-indentation probe is used, which can be used both for mechanical indentation, as well as current injection. The stress and strain applied on the sample can be recorded using a electrostatic transducer, and a piezo displacement sensor, similar to the PI95 holder. The electrical source meter has a mV and pA resolution in voltage and current.
Ideal use case: Samples can be studied under compression, or tensile stress. However, tensile stress requires the use of E-push to pull chips, and sample preparation often limits the ways in which this holder can be used. As with the PI95 holder, the samples may be imaged in bright field / dark field TEM, or via electron diffraction. It makes sense to study materials where the atomic structure or electronic structure can be tuned under strain. While the atomic structure can be studied through imaging / diffraction, the band structure changes are reflected in the I/V transport curves.
Compatible TEMs: JEOL 3010
23. Gatan 636 Cryo Non-transfer holder for JEOL
Description: The Gatan 636 double cooling holder is a Liquid Nitrogen based holder. The temperature can be set within a range of -170 to -100 °C using an external controller. Sample tilt range is limited to +/- 20 degrees in a and +/- 10 degrees on the b axis. Samples are fixed to the holder using a Beryllium hexring, and the holder can accommodate any TEM sample on a 3 mm grid. Similar to the furnace style heating holders, the entire sample is heated all at once. This makes the holder versatile, and capable of handling most conventional TEM samples. However, sample drift is significantly larger in such holders, and precise, hysteresis-free temperature control is not possible.
Ideal use case: The setup is ideal for studying phase transitions at low temperature, which may be observed via bright field TEM, or via electron diffraction. Often, damage in beam sensitive materials is mitigated by the use of a cooling holder.
Compatible TEMs: JEOL 3010
