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UHV Microscopy

Omicron Nanotechnology dual chamber multiprobe surface science system for in-situ preparation, modification and detailed analysis of various nanostructures and thin films in the ultra high vacuum (UHV) conditions.

 

Two main experimental techniques:

  • Electron Spectroscopy for Chemical Analysis (ESCA) for determination of the chemical composition of the sample,
  • Scanning Probe Microscopy (SPM) for measuring and imaging of the various surface properties with atomic resolution.
 

General features:

  • two interconnected chambers: first comprising the surface preparation units and ESCA, while the second one dedicated to support SPM techniques
  • multistage pumping system for acquiring the pressure of the order of 10-11 mbar inside both chambers
  • fast entry lock for quick sample and SPM sensors exchange
  • 5-degrees-of-freedom Omniax manipulator with cooling and heating stages for sample preparation, transfer and ESCA measurements

 

Variable Temperature Scanning Probe Microscope (VT SPM)

  • Scanning Tunneling Microscopy/Spectroscopy (STM/S) with sub-pA current operation
  • beam deflection Atomic Force Microscopy (AFM) for contact and non-contact measurements with the possibility to operate in various modes depending on the cantilever used (e.g. high resolution AFM, Electrostatic Force Microscopy – EFM,  Scanning Kelvin Probe Force   Microscopy – SKPFM and Magnetic Force Microscopy – MFM)
  • Q-Plus sensor combining AFM and STM
  • Matrix Control System
  • temperature control in the range of 30 ÷ 500 K
  • tip preparation tool for the in-situ conditioning of the STM tips
 
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Preparation of nanomaterials

Equipment:

  • Two fully transparent  gloveboxes (two- and five-gloves long) for manipulation of substances at inert atmosphere (argon, nitrogen or vacuum) with manually operated sluices
  • Muffle furnaces with heating up to 1100 oC and tube furnace with heating up to 1600 oC in controlled atmosphere
  • Autoclaves with teflon insides of various volume for carrying out the synthesis of nanomaterials in elevated temperature and pressure
  • Centrifuges of various speed (4000 to 28000 rpm)
  • Centrifugal evaporator
  • Rotary evaporators (Heidolph) with automatic temperature and speed controller, and manual vacuum controller
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Preparation chamber

  •  Single and Triple Electron Beam Evaporators (EFM 3 & EFM 3T), Organic Material Effusion Cell (OME40) and Low Temperature Effusion Cell (NTEZ) for the clean deposition of various atoms and molecules. Possibility of the controlled sub-mono-layer and multi-layer thin film growth with the use of Film Thickness Monitor (FTM)
  • atomic gas sources: Atomic Hydrogen Source (EFM-H) for passivation and Oxygen Atom Beam Source (OBS40) for controlled oxidation of the sample surface
  • Cold Cathode Sputter Ion Source (ISE5) for sample cleaning, depth profiling with ESCA and controlled induction of defects
  • Quadrupole Mass Analyzer (Quad 300) for residual gas analysis (vacuum purity and leak detection)
 

Surface profile Si (111) 7x7 along the marked line
 

Si surface (111) 7x7 imaged on two different voltage polarizations between the blade and the sample
 


STM. Surface Si (111), reconstruction 7x7, obtained by high-temperature processing in ultra-high vacuum (flash). Atomic resolution.

 

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Other equipment

  • Weighing scales
  • Mixer Mill Retsch MM400
  • Ultrasonic homogenizer
  • Freeze-dryer
  • Magnetic and mechanical stirrers
  • Spincoater
  • Diaphragm pumps
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Laboratory for work with hydrofluoric acid

The NanoBioMedical Centre has a special laboratory for work with hydrofluoric acid. The special application fume hood is dedicated for safe work with hydrofluoric acid
 

ESCA

  • multipurpose hemispherical energy analyzer SPHERA II
  • XPS with dual anode X-ray source (DAR 400) and monochromatic X-ray source (XM 1000)
  • UPS high intensity VUV source (HIS13)
  • AES electron source for 0.1 - 5 keV beam energies and spot size 300 mm (EKF 300)
  • electron source for charge neutralisation (CN 10)

 

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EPR imaging technique allows:

  • Spatial distribution of radicals in the sample (2D and 3D spatial imaging). In spectral-spatial imaging 2D, 3D, and 4D imaging is possible,
  • Monitoring mobility, polarity, molecular oxygen levels (pO2) and pH,
  • Monitoring of drug release from nanostructures, polymers etc.,
  • Study of diffusion of radicals in porous materials

Characterization of nanomaterials

Equipment:

  • Nitric Oxide Analyzer Sievers 280i
  • Transilluminator
  • Melting point meter STUART SMP10
  • Spectrofluorometer
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Advantages of EPR technique:

  • Enables the detection of paramagnetic centres: persistent radicals in biological materials, drugs, tissues, blood, and ions,
  • Enables the measurements of oxygen concentration in liquids especially blood by the use of dedicated radical spin probe,
  • Enables the study of spin dynamic in biological systems,
  • Is useful in the studies of ionizing radiation on biological samples. 

Example applications of EPR imaging:

PLA phantom of different shapes with 2.5mM TEMPO solution in water and reconstructed 2D image


Polidopamine powder in Nunc™ 15mL conical sterile polypropylene centrifuge tube and 3D (spatial) image reconstruction

 

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