Electron microscopy
Electron microscopy
Electron microscopy

Electron microscopy probes the structure, chemical composition and properties of materials on a local (even atomic) scale. The LMA has two TEM systems:

1) The Thermo Fisher Scientific Tecnai F30 is a very versatile high resolution Transmission Electron Microscope, capable of working in TEM and STEM (scanning and transmission) modes and equipped with all analytical techniques to obtain morphological, structural and compositional information of the sample with atomic resolution.
Working voltages for this microscope are 200 and 300 kV.

More information: https://lma.unizar.es/tecnai-f30/

2) The Thermo Fisher Scientific Tecnai T20 is a very versatile Transmission Electron Microscope, which can be used for both material science and biological samples.
The working voltages for this microscope are 200 and 80 kV and it is equipped with cryo-blades and low-dose software for image acquisition of extremely electron beam sensitive materials as well as for low temperature observation of vitrified materials (cryo-TEM).

More information: https://lma.unizar.es/tecnai-t20/

Applications: LMA

Titan microscopes (FEI Company) are 2 new generation microscopes incorporating a spherical aberration corrector (CEOS Company).

1) The Thermo Fisher Scientific Titan Image incorporates the corrector in the objective lens, which forms the image, making it the most suitable microscope for ultra-high resolution imaging (HRTEM). It also incorporates a biprism and a Lorentz lens for magnetic holography and high-resolution Lorentz microscopy.

More information: https://lma.unizar.es/titan-imagen/

2) The Thermo Fisher Scientific Titan Analytical incorporates the corrector in the condenser lens, which forms the incident probe on the sample. This makes it ideal for high-resolution scanning-transmission mode imaging (HRSTEM) and atomic resolution chemical composition mapping by electron energy loss spectroscopy (STEM-EELS). This microscope also incorporates a monochromator and a high brightness field emission gun (XFEG), which makes it especially interesting for the study of optical properties by low-energy EELS spectroscopy and the study of oxidation states by analyzing the fine structure of the absorption thresholds of EELS spectra.

More information: https://lma.unizar.es/titan-analitico/

The working voltages of this equipment are: 60, 80, 120, 200 and 300 kV. Being able to work at low voltage (60 kV, 80 kV) the corrector of these microscopes allows to obtain high resolution even in materials very sensitive to the electron beam such as graphene, carbon nanotubes or heteroatoms, zeolites and mesoporous materials, etc.

Applications: LMA

A Scanning Electron Microscope (SEM) is capable of imaging a sample by scanning it with a focused beam of electrons. The electrons interact with the sample producing different signals that are picked up by specific detectors and after their analysis, images of the topography of the sample and its composition are obtained.

The LMA has two pieces of equipment:

1) The Thermo Fisher Scientific INSPECT-F50 model field emission scanning electron microscope allows obtaining high resolution images of both secondary electrons and backscattered electrons as well as performing chemical analysis by x-ray energy dispersive spectroscopy (EDS).

More information: https://lma.unizar.es/sem-inspect/

2) The Thermo Fisher Scientific Quanta FEG 250 environmental scanning electron microscope (ESEM) is a field emission SEM. The ESEM Quanta FEG 250 allows working under three different pressure modes, the maximum pressure that can be obtained is 2600 Pa. This microscope allows the observation of biological samples, poorly conductive, without pretreatment since we can control the relative humidity of the chamber and the temperature of the sample to avoid damage during the observation time.

This equipment also allows increasing the temperature of the sample up to 1000 ºC, observing during the heating process the changes in the topography of the material. This scanning microscope allows the deceleration of electrons on non-conductive samples, obtaining resolutions of up to 1.4 nm, even using acceleration voltages of 1 kV.

More information: https://lma.unizar.es/esem-quanta/

Applications: LMA

The SAI also has the following equipment, which has the following specifications and instruments:

– Hot-tip field emission electron gun.
– Allows observations down to 0.8nm spatial resolution.
– Acceleration voltages between 0.02 and 30 kV
– Secondary and backscattered electron detectors in chamber and column (in-lens)
– EDS detector for energy analysis of X-Max (20mm2) scattered X-rays with Oxford Instruments SSD (Silicon Drift Detector) and energy resolution below 123eV at 5.9 KeV of Mn Ka.
– HKL EBSD (Electron Back Scatter Diffraction) Detector, Nordlys II, for recording and analysis of backscattered electron diffraction diagrams and crystallographic orientation maps. Processing with CHANNEL5 or AZtec.
– STEM detector
– Zeiss SIGMA cathodoluminescence detector SIGMA
– Fisheye” mode, which allows to have an image inside the camera.
– Silent mode” vacuum control system that periodically switches off the rotator in order to save energy and reduce noise in the lab
– Load compensation system by nitrogen injection. This system allows the observation of uncoated insulating samples using high-vacuum electron detectors.
– Plasma cleaning system, Evactron 25/45 from XEI Scientific, Inc.
– SmartSEM, AZtec, INCA, and Channel5 software
– ESPRIT DynamicS software for high-resolution EBSD pattern simulation.

Applications: SAI

Dual Beam (FIB-SEM) equipment is mainly used for nanolithography and lamella preparation processes. This equipment is located on two concrete platforms inside the clean room of class 10,000 (ISO7) and 125 m2.

The first Dual Beam equipment is the Helios 600 model, from FEI (now Thermo Fisher Scientific), which combines an electron beam (field emission source) accelerated up to 30 kV and a focused Gallium ion beam (working up to 30 kV). Both columns are positioned at 52º with respect to each other. The ion column is capable of working at low voltage (5 kV and below), which minimizes ion damage during lamella preparation. Five gas injectors are also available, thus allowing the growth of nano-structures with high resolution. For example, superconducting W nano-deposits with a lateral size of 40 nm and Co-based ferromagnetic nano-deposits with a lateral size of 30 nm, allowing to be at the forefront of research in these topics. In addition, it has a station of 4 electrical microtips (Kleindiek®) that are placed inside the chamber for in-situ electrical transport measurements and the possibility of carrying out electronic lithography processes thanks to Raith® hardware/software.

The second Dual Beam equipment located in the Clean Room is the Thermo Fisher Scientific Helios 650 model, which is an improved version of the Helios 600. The main difference between the two refers to the electron column, which has a monochromator and beam decelerator, reaching a resolution of 0.9 nm in the Helios 650. The ion column differs mainly from that of the Helios 600 in that it has a differential vacuum in the lower part, which allows a well-defined beam profile on the surface of the sample. The results obtained with this column show the possibility of growing materials of high scientific interest at the nanometer scale. In addition, this ion column is very suitable for the preparation of lamellae, in combination with the Omniprobe® nanomanipulator. The unit is also equipped with 5 gas injectors and a microtip station (Kleinkiek®).

Researchers from public or private centers as well as professionals from the industrial world who require the use of this equipment will also have, upon request, the scientific and technical support of our highly qualified and experienced staff.

In addition, a third dual beam or “Dual Beam” equipment is available, in this case cryogenic, the Thermo Fisher Scientific Nova 200 model. This instrument is mainly dedicated to the analysis of materials especially sensitive to electrons (“soft” materials). This instrument contains the core of the Nova Nanolab model 200, but has been upgraded with a cryogenic device that allows the study of materials at low temperatures.
The equipment therefore consists of a sample transfer device “cryo-transfer” together with a preparation chamber (cryo-chamber), which has an integrated system that allows to make a metallic coating on the samples through the “sputtering” technique. Thus, this instrument makes it possible to generate in situ fractures of soft materials, avoiding the damage associated with fractures made at room temperature.

More information: https://lma.unizar.es/dual-beam-helios-600-650/ and: https://lma.unizar.es/cryogenic-dual-beam-nova/

Applications: LMA

This microscope, acquired by CSIC in 2022, is considered to be the most powerful ultra-high resolution imaging and nanofabrication tool currently available. It has a unique and singular configuration at European level. It has three ion beams, Helium, Neon and Gallium, making it possible to use one or the other depending on the target. Specifically, the helium beam makes it possible to fabricate structures below 10 nm with a resolution of less than 0.5 nm.
The Orion Nanofab has an advanced and specific software for pattern design and application, NanoPatterning and Visualization Engine (NPVE). It also features a charge neutralizer that emits low-voltage electrons (Flood gun) to compensate the positive charge of semiconductor or insulator samples, facilitating their visualization.
In addition to these features, the following modular complements have been acquired and adapted to maximize the possibilities of use of this instrument, as well as the nature of the study materials.

– Cryo module (Quorum PP3010 cryo system): Maximum cooling temperature -190 C. Especially useful for soft samples. Allows low temperature fracturing. In conjunction with the gas injector allows the induced deposition of precursors, under cryogenic conditions, with 3 different ions (Cryo-FIBID).

– Precursor Injection System (Gas Injection System, Oxford): W, Pt and XeF2.
Allows the formation of deposits for structure protection, structure connection, direct writing processes of nanostructures or massive material removal.

– 4-microneedle station (Kleindiek): Enables electrical measurements of micro/nanostructures inside the microscope. They can also be used as nanomanipulators.

– Micro-heating/cooling plate (Kleindiek): Working temperature range from -55 to 125C. It allows working with the same material, at very varied and/or controlled temperatures to improve or study processes directly related to this property.

The use of these complements can be combined, which makes this equipment a particularly versatile microscopy and nanofabrication tool.

Contact: José María de Teresa (deteresa@unizar.es)

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