Microscopy laboratory

Atomic Force Microscope

  • Atomic Force Microscope Keysight Agilent 5500 works by scanning in contact, intermittent contact, and non-contact modes. Contact and intermittent contact modes work both in air and in liquid while non-contact scanning mode works only in air. The microscope can generate topography and phase contrast.
 

The microscope contains operating modes performed by the following attachable modules:

  • KFM (Kelvin probe microscopy), recorded simultaneously with the topography, with mechanical amplitude modulation - electrical amplitude modulation AM-AM and mechanical amplitude modulation - electrical frequency modulation AM-FM.
  • EFM used along with KFM for measuring dielectric films, metal surfaces, piezoelectrics, and conductor-insulator transitions
  • MFM (Magnetic Force Microscopy)
  • CSAFM (Current sensing force microscopy), useful in molecular recognition studies and can be used to spatially resolve electronic and ionic processes across cell membranes. 
  • PFM (Piezo force microscopy)
  • LFM (Lateral force microscopy), sometimes called Friction Force Microscopy Force spectroscopy (force - distance curves generation)
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  • Spectroscopie de forță (generarea curbelor forță-distanță)
  • STM (Scanning Tunneling Microscopy) with test cells and reference samples for each mode

Applications

Technical Specifications:

  • Equipped with 2 multi-purpose scanners which include independent piezo elements on +x, -x, +y, -y, z axes; Noise level: x, y <1A RMS, z<0.2A RMS for 9x9x2 microns operating area and x, y < 5A RMS, z < 0.2 A RMS for 90x90x8 microns operating area
  • Equipped with 2 STM-specific scanners
  • 8um (8x8x1.5), noise level: x, y <1A RMS, z < 0.2A RMS; nose cones sensitivity 0,1nA/ V ,1nA/ V standard, 10nA/ V
  • 1um (1x1x0.7), noise level: x, y < 0,6A RMS, z < 0.06A RMS; nose cones sensitivity 0,1nA/ V ,1nA/ V standard, 10nA/ V
  • Temperature control in air and liquid is offered with heating up to 250°C and cooling down to -30°C.

High Resolution Scanning Electron Microscope

The high-resolution Scanning Electron Microscope is equipped with a Schottky Field Emission source, which provides a clear, sharp, and noise-free imaging. In combination with the optimized analytical chamber geometry and its five-axis, motorized tilt, eucentric specimen stage, the high- and stable beam current (≤ 200 nA, continuously adjustable) makes this a tool well suited for (automated) short- and long-time EDS analysis and mapping. Typical applications include nano-characterization of metals and alloys, oxidation/corrosion, fractures, welds, polished sections, magnetic and superconducting materials, ceramics, composites, plastics, films/coatings, geological sections, minerals, soft materials such as polymers, pharmaceuticals, filters, gels, tissues, particles, porous materials, fibers.

- The electron source, the cannon, of the Inspect F50 microscope is emitting in a Schottky field.

– The maximum acceleration voltage is software controlled and varies from a minimum of 200V to a maximum of 30 kV.

– The sample current is 200 nA.

– The vacuum system of the Inspect F50 microscope provides a vacuum in the sample chamber of 6 × 10-4 Pa.-4 Pa.

– The vacuum system of the Inspect F50 microscope ensures that the working vacuum is reached after changing the sample in a maximum of 2.5 minutes.

The configuration of Inspect F50 includes:

– The resolution on the secondary electron (SE) image must be maximum 1 nm at 30 kV and maximum 3 nm at 1 kV.

– The detector system in the configuration of the Inspect F50 SEM microscope allows to obtain a resolution on the image of secondary electrons (SE) of 1 nm at 30 kV and 3 nm at 1 kV.

– Highly precision monitored eucentric and compucentric sample fixing platform in microscope configuration is software controlled after five axes: x, y, z, tilting and rotating, allowing movements that ensure the analysis of the entire surface of the samples:

  • Movement along the X axis: 50 mm (motorized, programmable by software)
  • Movement along the Y axis: 50 mm (motorized, programmable by software)
  • Movement along the Z axis: 50 mm
  • Tilting -10° – +70°
  • Rotation 360°

Transmission Electron Microscope (Crio TEM)

Titan Themis 200 is a scanning transmission electron cryo-microscope (cryoSTEM), equipped with field emission gun (FEG), having top performances in the following working modes: Transmission Electron Microscopy (TEM) and High Resolution Transmission Electron Microscopy (HRTEM), Scanning Transmission Electron Microscopy (STEM), Selected Area Electron Diffraction (SAED), CryoSTEM, 3D analysis in TEM and STEM modes, Energy Dispersive X-ray (EDX) microanalysis, Electron Energy Loss Spectroscopy (EELS), electron tomography in TEM. The advantages of this system, compared with other ones from the same class, are: high stability, controllability and reproducibility; field emission gun source (X-FEG), with high total current and lifetime; detectors system Super-X EDX, which makes possible the fast execution of analysis and elemental distribution maps; the 70° FOV Gatan system for cryo-transferring the samples (cross-sections or suspensions), frozen in the TEM holder at temperatures below -170°C. Additionally, transmission electron microscopy in cryogenic state of the samples contributes to the structural analysis for the beam sensitive samples (polymers, contaminated water, proteins, bacteria, sections of anatomic tissue, etc.).

Technical Specifications:

- Titan Themis 200 is a state-of-the-art, 80-200 kV FEG cryo Scanning Transmission Electron Microscope of the Titan family, which is designed to deliver the ultimate in performance in all TEM, STEM, and EFTEM modes.

- Titan Themis 200 can analyze at low temperature in all (HR)TEM, STEM, EFTEM, SAED, CBED modes as well as 3D in TEM and STEM modes.

- The Titan Themis 200 is equipped with revolutionary technologies such as:

  • Rigid construction, having a 300-mm diameter column featuring electron optics optimized for aberration correctors
  • ConstantPower™ design applied to all lenses that are critical in giving Titan its ultimate stability, and in enabling high controllability and reproducibility; 3 condenser lens system that extends the experimental parameter space with new options
  • X-FEG: FEI-designed high brightness Schottky field emission source which combines the benefits of Schottky FEG (high total current, great stability and long lifetime) with the brightness of a Cold FEG, without increased vacuum requirements or tip-flashing
  • Super-X EDX System: FEI’s proprietary EDX solution based on Silicon Drift Detector (SDD) technology. This provides superior sensitivity and unrivalled speed in EDX analysis and fast EDX mapping
  • STEM package: complete hardware and software package including a High Angle Annular Dark Field (HAADF) for fully digital STEM functionality

Performances

  • a vacuum system that is entirely oil-free
  • Adjustable voltage from the software, between 80 – 200kV
  • Piezo Enhanced CompuStage
  • Velox™ Software – the new FEI platform for signal acquisition, suitable for Windows 7, 64-bit
  • STEM resolution: 160 pm
  • Information limit: 90 pm
  • Point resolution: 90 pm
  • Super X EDS Spectrometer: detector resolution ≤136 eV for Mn-Kα and10 kcps (output)
  • High-visibility, Low-background, Double-Tilt, Super-X Compatible Specimen Holder
  • Ceta 16M, digital camera with 16 Megapixels
  • Gatan 70° Field Of View (FOV) cryo-transfer system
  • Low dose exposure technique
  • EFTEM EELS module
  • UltraFast EELS Spectrum Imaging
  • Lorentz lenses
  • Complete hardware and software for 3D analysis (tomography) for a tilt of +/ 70º
  • Software Amira for FEI systems

Dual Beam Scanning Electron Microscope for Biological Applications

The Dual Beam Scanning Electron Microscope for Biological Applications Versa 3D is a combination of two systems: a scanning electron microscope (SEM) with field emission gun (FEG) that produces enlarged images of a variety of specimens achieving magnification over 100 000× providing high resolution imaging in a digital format; a focused ion beam (FIB) system that is capable of fast and precise milling of the specimen material, revealing the structure under the surface layer, making cross sections, TEM lamella, deposition layers, etc. The ion system produces high resolution images as well.

This system also produces high resolution images. Users can switch between the two bundles for fast navigation and precise grinding. The tool provides optimal efficiency, resolution, and automation.

The instrument combines the enhanced electron and ion column with the most advanced ion beam lithography system.

- Vacuum

  • High-vacuum: <6×10--4 Pa
  • Low-vacuum: de la 10 la 200 Pa
  • ESEMTM mode: from 10 to 4000 Pa

- Source: Field emission gun assembly with NG Schottky emitter source.

- Voltage: 200 V to 30 kV (50 V landing energy possible with Beam Deceleration)

- Resolution:

  • High-vacuum mode: 1 nm at 30 kV and 2.3 nm at 1 kV (SE); 2.5 nm la 30 kV (with DBS)
  • Low-vacuum mode: 1,5 nm at 30 kV and 3 nm at 3 kV (SE); 2.5 nm la 30 kV (with DBS)
 

– Ion optics: Field emission focused ion beam optics with liquid Gallium ion emitter.

Source lifetime: minimum 1000 working hours

- Voltage: 500V ÷ 30 kV

- Beam current: 1.5 pA to 65 nA in 15 steps

- Resolution: 7.0 nm at 30 kV at coincidence point, 5.0 nm at optimum working distance

- High precision 5-axes motorized stage

  • X,Y: 150 mm, piezo-driven
  • Z: 10 mm (motorized)
  • T: from -10° to +60°
  • R: n x 360°, piezo-driven
  • X, Y repeatability: 1.0 μm

- Detectors

  • Everhart-Thornley SE detector (ETD)
  • IR camera for viewing sample/column
  • Chamber integrated Nav-Cam+™
  • High performance Ion Conversion and Electron (ICE) detector for secondary ions (SI) and electrons (SE)
  • Retractable Directional Backscatter (DBS)
  • In-column Detector (ICD)
  • Retractable WET-STEM detector with BF/DF/HAADF segments and Peltier stage (-20°C ÷ 60°C)
 

- Accessories

  • Gas Injection System (GIS)
  • GIS – Beam chemistry options
  • In situ sample lift-out system (Omniprobe™ 100,7, AutoProbe etc.)
  • Plasma Cleaner (PC)
  • Beam Deceleration (BD) mode
  • Charge Neutralizer
  • Integrated Fast Beam Blanker
  • EDS: integration kit (EDAX) 
  • Exclusive cryo solution for DualBeam
 

– Software:

  • AutoSlice and View™ – automated sequential mill and view to collect series of slice images for 3D reconstruction
  • AutoTEM™ wizard - automated sample preparation with section wizard for fast, repeated, reliable, automatic ion beam sectioning in one or more user-defined sites of ultra-thin blades for TEM analysis.

RAMAN microscope

The Raman LABRAM HR Evolution microscope from Horiba is a confocal microscope for high performance, used for making non-destructive spectral analyses, with very good spectral and spatial resolutions, with UV-VIS (ultraviolet-visible) and NIR (near-infrared) options, with the capability of making automated single point analysis and multi-point analysis. The LabRAM HR Evolution is prepared for UV analyses with its included optics and ensures a transmissibility of the optical signal in the spectral range 200 – 2100 nm and includes a module (remote) Raman coupled optical fibers for non-contact measurements remotely (for 633 nm) and an accessory (MACRO-CH) for determination of the Raman of liquids in vats with multipass effect to ensure the increasing intensity of the signal.

The instrument can:

  • measure the Raman spectra with a spectral resolution of at least 1.5 cm-1-1 in UV (measured as full width at half maximum (FWHM) for the 365.015 nm line of the mercury lamp, using a diffraction grating of 2400 g/mm);
  • measure the Raman spectra with a spectral resolution of at least 0.6 cm-1-1 in the visible range (measured as FWHM for the 585 nm of the neon lamp, using a diffraction grating of 1800 g/mm);
  • measure the Raman spectra with a spectral resolution of at least 0.3 cm-1-1 in near infrared (NIR) (measured as FWHM for the 837.76 nm line of the neon lamp, using a diffraction grating of 1800 g/mm).
 

The system has the following laser wavelengths, but also the optical and mechanical configurations for using these lasers:

  • 633 nm, 17 mW
  • 488 nm, 120 mW
  • 514 nm, 120 mW
  • 785 nm, 100 mW
 

The system allows further upgrade with additional lasers wavelengths in the UV, in visible or in infrared (325 nm, 532 nm, 830 nm, 1064 nm), switching between lasers, controlling the intensity of the laser power through the use of neutral density filters (with a motorized swivel support that has 9 positions: 100%, 50%, 25%, 10%, 5%, 2%, 1%, 0.1%, 0.01%), which are controlled by the software, the selection of the diffraction gratings (delivered with 2 diffraction gratings: 600 g/mm and 1800 g/mm, and the selection of rejection filters is completely automatized and software-controlled.

Filters

  • The filters are stable in time, being a polymer type and they don’t place artifacts in the spectral measurements (especially at low frequency).
  • The filters included in the configuration are Edge filters to provide maximum sensitivity, the filters operate in the mode of injection/rejection; the same filter reflects the light into the microscope and rejects the Rayleigh signal and the scattered light, that is reflected into the spectrometer.
  • The filters allow measurements up to 50 cm-1 for visible and NIR (for 488 nm wavelengths, 512 nm, 633 nm, 785 nm) and up to 150 cm-1 in UV (for 325 nm wavelength).
 

Detector

  • CCD detector with a 25-width chip and at least 1024x256 pixels. In order to acquire data both in stationary and in continuous scan mode, without spectral distortions, it is used the complete chip (1024 pixels). The resolution is kept constant throughout the chip.
  • cooled with liquid nitrogen for a low level of noise, with the front lit variant, which provides sensitive spectral domain between 200 and 1050 nm with a quantum efficiency of 40% between 200 nm and 900 nm, low noise, and darkness noise of 0.001 e/pixel/sec.
  • directly coupled to the spectroscope (not connected through fiber optics), open (open microscope) and allows analyses on large samples; focusing is done by moving the lens of the microscope, not the sample.
  • completely and permanently integrated to the system, providing spatial resolutions, susceptibilities, and very good stability.
  • spatial lateral resolution is 350 nm in the visible (488 nm laser excitation);
  • confocal axis resolution, at least 1.5 μm in visible.
 
The confocal microscope
 
  • The system ensures a confocal volume that can be varied continuously and automated through a large aperture (NA >0.5)
  • equipped with a color USB video camera for the viewing of samples by white light illumination and laser spot at the same time.
  • equipped with the following objectives: 10x, 50x and100x
 
Heating/cooling cell
 
  • The system includes an accessory to analyze samples in a cell (heating/cooling cell), which allows temperature control through software, between - 196°C and 600°C. The cell is adapted for transmitted and reflected light.
  • sample area: diameter of 22 mm;
  • cell size: 137 x 92 x 22 mm;
  • water cooling for measurements at high temperatures.
  • liquid nitrogen cooling for measurements at low temperatures
 
Hiperspectral images
 
  • The XY stage is motorized and coresponds to the obtaining of hiperspectral images at a high spectral resolution (dimensions: X = 75 mm, Y = 50 mm).
  • The system allows XY automated mapping, with the following technical features:
  • software controlled;
  • the step is better than 0.05 microns on XY and 0.1 microns on Z axis.
  • The scanning system (DUSOCAN) is dual for UV, VIS and NIR and can operate in two modes: scanning mode and collection of the Raman signal on a large surface, avoiding damage to the photosensitive materials and a step-by-step mode for acquisition of Raman spectra in points for sample mapping, resolution step of 50 nm.
 
The sample remains coupled to fiber optics for non-contact remote measurements
 
CH accessory - for determination of the Raman of liquids in vats with multipass effect to ensure the increasing intensity of the signal (focal length 4 cm, 1 x 1 cm vat).