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PHI 5000 VersaProbe
 
 PHI 5000 VersaProbeTM - Scanning ESCA Microprobe? (ULVAC-PHI, Japan/USA, 2008) is a base a new surface analysis system, partially financed by European Regional Development Fund ERDF in the Sectoral Operational Programme ?Improvement of the Competitiveness of Enterprises SOP ICE, years 2004-2006?
The PHI VersaProbeTM is a unique scanning X-ray monochromator XPS instrument that provides outstanding micro-spectroscopy analytical performance. The PHI VersaProbe includes a focused and scanned X-ray beam for sample imaging and analysis, a spherical capacitor energy analyzer with multi-channel detection, a high performance low voltage argon sputter ion gun, a unique charge compensation system and a large travel five axis precision sample stage. The PHI VersaProbe provides X-ray excited secondary electron imaging of the sample surface in a manor analogous to how a SEM generates a secondary electron image. This unique feature utilizes the scanned X-ray beam to generate secondary electrons that are collected by the energy analyzer to provide images of the sample topography, morphology and other features. This guarantees that spectroscopic data is collected from the selected feature of interest.
The PHI  VersaProbeTM  is equipped with a unique dual beam charge compensation system that utilizes both a cool cathode electron flood source and the very low energy ion capability of the argon ion sputter gun to provide turnkey neutralization of all sample types.


The high resolution 180 spherical capacitor energy analyzer provides full-featured XPS analysis capability including XPS spectral, map, depth profile, line scan and angle-resolved analysis. The 16 channels multi-channel detection system provides high sensitivity and high dynamic range.  Because the analysis area is defined by the X-ray probe instead of analyzer apertures, the PHI VersaProbeTM has unequaled micro-area spectroscopy capability. X-ray induced sample damage is also minimized as only the area of analysis is irradiated with X-rays.

The five axis computer driven motorized sample stage provides a stable analytical platform with high degrees of accuracy and reproducibility.  X and Y translation of ? 25 mm allows sample holder to be accessed with rotation. Z translation of 20 mm and tilt of -45? to 45? are included. Sample holder can be cooled/heated etween -1001000 C. Multiple sample positions can be stored by the computer for automated, unattended analysis of multiple samples. Zalar? and Compucentric Zalar? sputter depth profiles provide enhanced interfacial resolution through the minimization of sputter artifacts by precise sample rotation.

Ultra-High Vacuum analytical chamber, analyzer, scanning X-ray source, C60 ion gun, UV source,
AES electron gun


Ion gun,  motorized  sample stage,
Dual anode X-Ray Source, optical microscope
The C60 ion gun can be adapted to provide surface cleaning capability, maintaining the chemical states of polymer samples. This unique feature also allows sputter depth profiling for such as polymer thin films with monolayer resolution. The C60 powder is evaporated and injected into an electron impact ionizer. The C60 ion beam is accelerated through the extraction lens which focuses the beam at the Wien filter aperture for mass separation. The isolation valve is integrated for source maintenance without breaking vacuum of analytical chamber. The ion gun column has a 1 degree bend at the blanking plate for eliminating neutral particles to preserve sample chemistry, enhance depth resolution and minimize sputtering of adjacent areas. 

The original PHI VersaProbe (TM) apparatus was combined with complex UHV system provided by Prevac. The construction of this system allows a sample preparation and a complex surface analysis to be performed in situ in UHV condition. The system is equipped with: XPS-UPS (PHI VersaProbe) and STM/AFM  (RHK Technology) analytical chambers, high pressure flow reactor and multicapable preparation chamber, which contains: precise manipulator, electron beam evaporator, effusion cell, quartz oscillator, LEED (OCI Microengineering), quadrupol mass spectrometer (Stanford Research), cleaning ion gun and palsma source (SPECS).
  The flow through high pressure reactors are a chamber with equipment designed to affect a sample by gases at high pressure (up to 20 bar) and carry out pressure experiments. In that flow through high pressure reactor, only the sample and parts of the sample holder are in contact with the reaction gas. The flow through high pressure reactor is equipped with connecting flanges in UHV standard different sizes for connecting current and further equipment. Vacuum in a reactor chamber reaches a value of below 1x10-8 mbar. Reactors with cooling and heating options can work in a range of temperatures from -100C to 650C

STM/AFM chamber High pressure reactor chamber
Load lock and preparation chamber
Distribution chamber

Highly advanced preparation chamber is designed for preparing the samples for scientific research and for an initial analysis by AES, LEED and TDS. Chamber is equipped with:
  • 5 Axes Precise manipulator X, Y, Z, R1, R3 with R1. Manipulator is equipped with the Sample Receiving Station for holding sample holders. The station allows to heat up samples in controlled manner up to 1200oC as well as cool it with liquid nitrogen. Manipulator is controled with PREVAC control software.
  • LEED-AES spectrometer with microchannel plates.
  • Ion Source IS40C1 for surface cleaning.
  • Quartz oscillator TM-400 on sample holder.
  • Multi gauge controller MG13 for complete UHV pumping system including pressure measurement.
  • Viewports.
  • Electron beam evaporator EBV40A1 for sub-monolayer and multilayer thin film growth by molecular beam epitaxy.
  • Effusion cell EF40C1 with indirect resistive heating for sub-monolayer and multilayer thin film growth by evaporation/sublimation.
  • Residual gas analyzer RGA300 with process controller EUROTHERM 2408 for thermal desorption (TDS) and analysis of residual gases in the preparation chamber.
  • Gases dosing system of different gases (Ar, H2, O2, etc.)

Moreover the system is equipped with sample loading, transferring and storage system, equipment for the sample preparation and  cleaning, gas dosing system, pressure and temperature measurement and control system, vacuum controlling system, sample temperature measurement and control system, sample loading, prepared for UHV transport box usage, unique Radial Distribution Chamber system with extremely easy handling solution, storage chamber with possibilities for samples heating and cooling, solution with extremely short time heating in high pressure and UHV.

Our Vacuum Transport Box designed for transporting samples between different UHV systems in ultra high vacuum conditions. Samples placed in sample holders may be stored and transported inside the transport box without changing pressure level. To maintain the inner vacuum conditions the transport box is equipped with an ion pump and measuring device. The pump is designed so that it can to be powered e.g. from a car battery or from other power source. Vacuum is up to ~10-9 mbar.

 

Software

We use the following software to process our experimental data:

  •  ECLIPSE (VG Scientific Equipment Data System) for processing data recorded on ESCALAB-210. The OS/2 WARP/e-ComStation based software.
  •  The Avantage Data System for Thermo VG Scientific equipment controls all aspects of data acquisition and used to processing data recorded on ESCALAB-210 and MICROLAB-350 using comprehensive set of data processing tools.
  •  PHI MULTIPAK. MultiPak is a complete data reduction system for Auger and XPS spectra. Software is used for processing data recorded on PHI 5000 Versa Probe.
  •  CasaXPS. Processing software for XPS, AES from Casa Software Ltd. Could process results from all our spectrometers and most used techniques.
  •  UNIFIT v. 2009. Spectrum Processing, Analysis and Presentation Software for Photoelectron Spectra.
  •  QUASES. Quantitative Analysis of Surfaces by Electron Spectroscopy, written by Sven Tougaard (QUASES Tougaard Inc). Software Package for quantitative XPS or AES analysis of three dimensional surface nano-structures.
  •  Multiline v. 2.0. Software developed in Institute of Physical Chemistry by prof. A. Jablonski, use more then standard set of peaks, for increasing precision of quantifications.
  •  EPESWIN Software developed in Institute of Physical Chemistry by prof. A. Jablonski, can be applied for improvement of IMFP results.
  •  XPMPro Software used to control SPM microscope and to proceed obtained data.
  •  Gwyddion.net Program for SPM data visualization and analysis with highly advanced visualization and statistical module.
  • QUASES-ARXPS quantitative analysis of the surface by electron spectroscopy, written by Sven Tougaard (QUASES Tougaard Inc). Software package for quantitative XPS/AES of surface nanostructures by analysis of the variation of peak intensities with emission angle.
  • xT microscope control, EDAX Genesis, WDS shell Software package for SEM microscope control, data aquisition, processing and presentation. Could process EDS and WDS spectra.

We use advanced databases, developed with our Institute cooperation and offered by National Institute of Standards USA ? (NIST):
  • NIST Standard Reference Database 64 - NIST Electron Elastic-Scattering Cross-Section Database: Version 3.1 (F. Salvat, A. Jablonski)
  • NIST Standard Reference Database 71 - NIST Electron Inelastic-Mean-Free-Path Database: Version 1.1 (C.J. Powell, A. Jablonski)
  • NIST Standard Reference Database 82 - NIST Electron Effective-Attenuation-Length Database: Version 1.1 (C.J. Powell, A. Jablonski)
  • NIST Standard Reference Database 154 - Backscattering-Correction-Factor Database for Auger Electron Spectroscopy, Version 1.1 (A. Jablonski, C.J. Powell)


For peak identifications we use:

  • NIST Standard Reference Database 20 - NIST X-ray Photoelectron Spectroscopy Database: Version 4.1
  • Handbook of X-ray Photoelectron Spectroscopy ? J.F. Moulder, W.F. Stickle, P.E. Sobol, K.D. Bomben ? ULVAC-PHI, 1995, also our own rich literature database.


  Sample requirements

Only solid state material can be analysed, which is stable in ultra high vacuum conditions. Porous samples and materials contaminated by high vapour pressure solvents (ceramic, polymers) should be preliminary drying (e.g. by stoving or vacuum drying) and saved in vacuum vessels or in containers filled by inert gas (N2, Ar).Only conducting samples can be analyzed by AES. The samples, which contain such elements like Hg, Zn, J, Te, Cs, K, Na, As, Ga, Ca, S, P can be analyzed only if these elements are chemically bonded, because of potential danger of analytical system damage. The best size of solid state samples is 10 x 10 mm (acceptable size within a range: from 1 x 1 mm to 30 x 30 mm) and thickness lower than 10 mm. Powder samples net weight should be higher than 100 mg. Sample size requirements for scanning probe microscope slightly differs from above. Please contact us if you need additional information.

Photoelectron spectrometer ESCALAB-210

  The spectrometer ESCA-XPS (X-ray Photoelectron Spectroscopy) contains automatic system of data acquisition, processing and analysing. The spectrometer consists of pre-processing chamber which allows sample pre-treatment under controlled conditions of pressure (to 0.5 bar) and temperature (from -160o to 800o C); gate enabling quick direct sample transfer to the analysing chamber; basic analysing system consisting of photoelectron source with double anode (Mg and Al) working alternatively; pumping system to obtain ultra-high vacuum; electronics and computer with the spectra acquisition, processing and analysing system. The sample surface cleaning procedure removing the contamination of the investigated material surface layer is proceeded by an Ar+ ion source (AG21) in the analysing chamber.
Base system comprisies: double focusing spherical sector analyser, electrostatic input lens with iris mechanism, 5 channel electron multipliers, 4 axis manipulator, dual anode X-ray source, selected area XPS aperture system (Large Area  2x6 mm, 1mm, 600?m, 300 ?m, 150 ?m, 60 ?m), AG21 cold cathode ion source (10 keV). The system was systematically upgraded and modernized in time of its using. At present the spectrometer is equipped additionally with: preparation chamber, suitable for cooling/heating in range -100 to 1600C, ion gun for cleaning samples, 3-gas admission system with Barocell pressure transducers. Original Posiloc sample holder is changed to PTS sample holder system (PREVAC).
A flood gun for charge neutralization and residual gas analyser (200 amu) were installed in the analytical chamber, giving possibility to programmed thermal desorption analysis. Original DEC PDP-11/53 hardware with a VGS data-system software is changed to ECLIPSE data-system working on PC computer.
Load Lock chamber is now pumping by dry and small turbomolecular pump for preventing surface of samples from possible oil vapour contamination. Preparation chamber is pumping by turbomolecular pump, analyser chamber is pumped both by ion and sublimation titanium pump.

Scanning Electron Microscope
Nova NanoSEM
450

The FEI Nova NanoSEM 450 Scaning Electron Microscope is an advanced nanoscale research tools for a wide range of applications. Spectacular results are consistently obtained on a variety of challenging materials, in particular nanoparticles and powders, nanotubes and nanowires, plastic electronics, glass substrates, organic materials, diamond films and more.

Nova NanoSEM 450 key benefits are:
  • Field emission SEM with ultra-stable, high current Schottky gun
  • Beam landing energy: 50 eV - 30 keV
  • Advanced optics and detection, including immersion mode, beam deceleration, in-lens -SE and -BSE, DBS and STEM for best selection of the information and image optimization
  • Resolution:
-  0.8 nm at 30 kV (STEM)
-  1.0 nm at 15 kV (-SE)
-  1.4 nm at 1 kV (-SE) without beam deceleration
  • True high resolution in low vacuum FESEM: 1.8 nm at 3 kV and 30 Pa
  • Beam current up to 200 nA for analysis in high or low vacuum
  • Ultra-clean, oil free scroll- and turbo-pumped vacuum system
  • 110 x 110 mm high precision stage

Two basic operation modes of Nova NanoSEM 450 are low and high vacuum. The typical pressure value for HiVac mode is 6.10-5 Pa where as in LoVac mode pressure ranges from 10 to 200 Pa. Turbo Molecular Pump backed by a scroll pre-vacuum pump, obtains the necessary specimen chamber pressure. Low vacuum capabilities are unique and allow to study most non-conducting or contaminating materials. Observation of such samples could be made without the need to metal coat the sample, which would be necessary for conventional high vacuum mode. Microscope is supplied with multiple detectors fitted for low vacuum mode (LVD, Helix, GAD) to obtain high resolution images in such conditions.
The Nova NanoSEM 450 has a computer-controlled high-accuracy five-axis stage. It offers precision specimen computer controlled manipulation and automation of all axes. Additionally Navigation HD camera and a correlative navigation unit help to find and move to the right region of interest in no time. Spacious microscope chamber allow us to study reasonable big samples.

EDX (Energy-dispersive X-ray) and WDX (Wavelength dispersive X-ray) spectroscopes are the parts of the system. Those techniques allow to study samples qualitatively and quantitatively, perform local chemical analysis, draw elements distribution maps.
Microscope is additionally equipped with:
  • FEI Plasma cleaner - plasma source designed to clean microscope chamber and samples.
  • FEI Cryocleaner - contamination trap cooled with liquid nitrogen.
  • Quick loader system - besides to the regular multisample holder system is equipped with Quick loader. This system allows us to change the sample within 2 minutes without need to open microscope chamber. Software and interlocks protect the system against damage.
The FEI Nova NanoSEM 450 was financed by the Project FP7-REGPOT-CT-2011-285949- Noblesse.

Scanning Auger Microanalyzer
Microlab 350

Microlab-350 is equipped in a Schottky-type field emission electron source. The electron column is capable of producing a spot size < 7nm at the Auger analysis position at a current of 1nA and electron energy 25 keV. The spherical sector analyser has a user-selectable energy resolution in the range 0.02% to 2%.The detector is an array of 6 channel electron multipliers. Spectrometer have a fully motorized sample manipulator with 5 axes of movement. The fifth axis, continuous rotation, is used during sputter depth profiles, conducted by EX05 ion gun. High magnification SEM images can be produced  using the Secondary Electron Detector. Additionally, twin anode X-ray source, with digital X-ray power supply, is fitted to the instrument. Another installed option is sample impact fracture stage on the fast entry chamber. The analytical chamber is pumped both and ion pump and titanium sublimation pump, allows to achieve a vacuum better than 5 x 10-10 mbar.
All system is under the Avantage, Windows?based data system, which control all aspects of data acquisition: sample aligment, analyser lenses, detector, X-ray source, field emission electron gun, ion gun. Avantage has also a comprehensive set of data processing tools as peak identification, peak fitting, quantification, non-linear least squares fitting, depth profile and another.

  Microlab 350's key features are:

  •   SEM-Scanning Electron Microscopy, spatial resolution: < 9 nm at 25 kV
  •   SAM-Scanning Auger Microscopy, lateral resolution < 20 nm at 10 kV, depth resolution 0.5 ? 2 nm (local chemical analysis: qualitative and quantitative, surface distribution of the elements, linear distribution of the elements)
  •   High sensitivity, detection of the elements ~ 0.5 at.%, the range of the analyzed elements from lithium (Z=3) upward 
  •   User selectable energy resolution 0.6% - 0.06% (local identification of the chemical state of the elements)
  •   Determination of the depth distribution profiles of the elements with nanometric resolution, combined with the function of ion etching
  •   Multi-technique capability (AES-Auger Electron Spectroscopy, XPS-X-ray Photoelectron Spectroscopy)
  •   Avantage software, a Windows based data system for recording and processing data
  • The Microlab 350 is a high-performance scanning Auger instrument using field emission technology to provide high spatial resolution. The spherical sector analyzer (SSA), used on Microlab 350, allows the analysts to select the best combination of energy resolution and sensitivity for each analysis, in common with most other spectroscopic techniques. Microlab 350 additionally is equipped in:
  •   X-ray gun (twin anode source: AlK?, MgK?) for XPS measurements (spatial distribution: average value from all sample surface area); this extends the use of this instrument to (X-ray Photoelectron Spectroscopy) dielectric materials
  •   Ion gun for sputter etching; usually ion gun is used for depth profiling, sample cleaning and charge compensation.
This instrument is particularly useful to investigate small surface features, thin layers, impurities in materials as well as to determine their chemical (elemental) composition and chemical state of their components.
The apparatus is equipped with UPS (COMEX) power supply.

  Sample preparation for surface analysis
Samples cannot exceed 15 mm in a diameter and 8 mm in height. AES technique is limited to conducting materials: metals and semiconductors of sufficient conductivity. The stability of samples in the ultra-high vacuum conditions is required (the pressure lower than 10-10 mbar).
Additional equipment used in preparation of the samples: stereo microscope, laboratory dryer (max. temperature: 250C), the heating furnace (max. temperature: 1100C), Autoclave - steam sterilization of the metal surfaces under pressure.

  Restrains
Samples containing elements such as Hg, Te, Cs, K, Na, As, J, Zn, Se, P, S, etc. or their compounds cannot be analyzed because of a possibility of analyzer damage. The same concerns the samples which decompose with emission of compounds such as H2O, HCl and H2S under conditions of ultra-high vacuum and/or X-ray radiation.

Spectrometer XPS/AES
VG Microtech

  The spectrometer, equipped with the twin anode (Al, Mg) X-ray source and the electron gun LEG62, allows use the X-ray Photoelectron Spectroscopy (XPS) and the Auger Electron Spectroscopy (AES) techniques for chemical analysis of surface and thin film characterization. The emitted electrons are analysed by the hemispherical electron energy analyser CLAM2. The low energy ion gun AG5000 allows not only for sample cleaning, but also for the depth-profiling analysis of the surface films.
The chamber is consecutively pumped using a rotary vacuum pump, a turbomolecular pump, a titanium sublimation pump, and an ion pump. This arrangement allows quickly achieve a vacuum of 10-9 mbar.
A simple Windows compatible computer system gives user-friendly data acquisition. Then, the obtained XPS/AES spectra can be processed and analysed using commercially available software.
The VG Microtech system is relatively simple. It is easy to familiarize with its devices and to understand the principles of XPS and AES. For these reasons, the VG Microtech Spectrometer can be especially useful for teaching purposes.

Electrochemical System for Corrosion Studies Autolab PGSTAT302N

Autolab PGSTAT302N - for electrochemical investigations, providing major electrochemical methods including Electrochemical Impedance Spectroscopy (EIS).