Cryogenic Dual Beam-Nova

by | Nov 25, 2021 | Microfabrication: Dual Beam and Microchatacterization, SEM, XPS, and CRD areas

OPEN COMPETITIVE ACCESS

ACCESS ON DEMAND (always available, with fee)

The cryogenic dual beam instrument is dedicated mainly to analysis of electron-sensitive materials (soft materials). The equipment core is based on the Nova Nanolab 200 model, but upgraded with a cryo-setup that allows the analysis of materials at low temperatures. This capability consists of a cryo-transfer setup and a cryo-chamber with embedded sputtering system. For example, this system permits to in situ generate controlled fractures on quenched soft materials, avoiding the mechanical damage associated with room temperature fractures.
In addition to the study of the material in its original state (porosity, embedded nano-objects, internal heterogeneities, etc.), any internal distribution of materials can be determined by using the Focused Ion Beam (FIB) to produce cross-sectional surfaces. A combined strategy between this equipment and the Helios Dual Beam Model 650, also available at our Center, is being conducted to produce series of ion-cuts of biological materials embedded in epoxy. These images are being used to produce three-dimensional (3D) information of material distributions. Appropriate software for compositional analysis based on Energy-Dispersive X-ray micro-analysis (EDX) is also included in this equipment. Additionally, the equipment also holds an Omniprobe nanomanipulator for lamellae preparation as well as 5 gas injectors.

The expertise of our scientific and technical staff is also offered to researchers from public and private research centers and also to professionals from industrial sectors that require the use of this instrument.

Image (resolution 1.4 nm)/ Analysis:
By using the different detectors available within this instrument, the following information can be obtained:
  • Image with secondary electrons and topography by means of an ETD/TLD (Everhart-Thornley/ Thru-the-Lens Detectors).
  • Image (back scattered electrons) and composition by using a BSED (Back Scattering Electron Detector).
  • Image with secondary ions, sensitive to crystallographic direction.
  • Elementary Chemical Analysis by EDX (Energy-Dispersive X-ray micro-analysis).
  • STEM (scanning-transmission) images.
Nanofabrication (lateral dimension between 50 nm and tens of microns)
  • FIB: focused ion beam; etching of a predesigned motif over the sample.
  • FEBID/FIBID: focused electron/ion beam induced deposition.
PRECURSOR GASES
(CH3)3(CpCH3)Pt, Co2(CO)8, W(CO)6, TEOS + H2O –> SiO2, Selective Carbon Mill (MgSO4·7H20)
Micromanipulation
  • Lamellae preparation in conventional mode.
  • Thinning at low temperatures (samples for TEM observation).
  • Nano-manipulator (Omniprobe).
Low Temperature
  • Fast freezing and cryo-fracture of materials. Samples can be fractured in the -180 to -150 ºC range. The observation can be made between -130 and -140 ºC ± 1 ºC.
  • Non-conductive samples need metallization, which can also be done in our Centre.
  • Conductive and non-conductive samples as bulk, films, powder (compacted), etc. can be studied.
  • Samples should be compatible with high vacuum conditions.
  • Samples in the 1 mm to 100 mm range can be studied. They should be less than 10 mm thick.
  • Use of the cryo-option allows the measurement of liquid samples, semi-liquids and beam sensitive samples, polymers, resins, MOFs (metal-organic frameworks), etc.
Electron beam resolution
2.5 nm at 1 kV, 1.4 nm at 15 kV
Ion beam resolution
7 nm at 30 kV
Landing Voltage Range
E-beam: 200 V-30 kV
I-beam 2kV-30kV
Probe current
E-beam 1.4 pA (1kV) up to 37 nA (30kV)
I-beam: 1 pA up to 20 nA at 30 kV
High Precision
5-axes
motorized stage
XY: 50 mm
Z: 25 mm
T: -10 to +60
R= 360° (continuous)
Chamber
vacuum
<2.6 x 10-6 mbar (after 24 h pumping)
Sample Size
Maximum size: 150 mm diameter with full rotation( larger samples possible with limited rotation).
Weight: max 500 g (including the sample holder).
Cryo-option
Model PPT2000 with Cryo-transfer from Quorum Technologies
Transfer
After freezing and vacuum transfer the sample is placed on the preparation chamber cold stage. Stage temperature is normally set to between -130oC and -140oC (precisely controlled to with +or- 1C)
Fracturing
Sample can be fractured using either the cooled probe or cryo knife Tools.
SUBLIMATION (ETCHING):
Water (ice) can be sublimed (etched) from the sample by raising the stage temperature (typically to between -80oC and -100oC.
COATING
Sample is sputter coated with Pt or C and then transferred in to the SEM cold stage.

a) Pt deposited by e- over multilayer organic magnetic tunnel junctions b) View of milling by i+ beam during the process to make lamella previous to the lift out.

a) Electron image of lamella of organic magnetic tunnel junctions on the grid. b) Final view of the lamella, ion image c) details and thickness of lamella by ion image, the final process was made at low temperatures (-160 ºC)

(A) General overview of polymers after cryofracture. (B) Details about the internal structure and distribution of Zeolite. (C) Show the spectral analysis of specific zeolite areas, demonstrating the presence of the aluminum and Silicon typical in the zeolite.

a) Pt deposited by e- over multilayer organic magnetic tunnel junctions b) View of milling by i+ beam during the process to make lamella previous to the lift out.
a) Electron image of lamella of organic magnetic tunnel junctions on the grid. b) Final view of the lamella, ion image c) details and thickness of lamella by ion image, the final process was made at low temperatures (-160 ºC)
(A) General overview of polymers after cryofracture. (B) Details about the internal structure and distribution of Zeolite. (C) Show the spectral analysis of specific zeolite areas, demonstrating the presence of the aluminum and Silicon typical in the zeolite.

Laboratorio de Microscopías Avanzadas

We are a unique initiative at national and international levels. We provide the scientific and industrial community with the most advanced infrastructures in Nanofabrication, Local Probe and Electron Microscopies for the observation, characterization, nanopatterning and handling of materials at atomic and molecular scale.

Contact information

Campus Río Ebro, Edificio Edificio I+D+i

C/ Mariano Esquillor, s/n
50018 Zaragoza (España)

Tel.:(+34) 976 762 980
lma@unizar.es

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