technician working in a glovebox


Equipment available at the Department Micro- and Nanostructures

Electron and Ion Microscopy / Film Analysis

TEM Titan3 Monochromated, Double Cs-Corrected

Description follows

TEM Tecnai F30

(300kV, FEG, TEM/STEM, GIF, EDX, HAADF, CCD)

Our transmission electron microscope Tecnai F30 (from Philips -> FEI Company -> Thermo Fisher Scientific)

Operates at 300 kV accelerating voltage and is equipped with:

  • Field emission gun (FEG)
  • Super-twin alpha objective lens
  • Scanning unit (STEM) with bright field (BF), dark field (DF), and high angle annular dark field (HAADF) detector
  • Energy dispersive X-ray spectrometer (EDXS) (Edax/Ametek TEAM Octane T Optima EDS windowless)
  • Imaging energy filter (Gatan GIF 200)
  • Multiscan CCD camera (Gatan MSC 794)
  • Integrated programmable user interface for all components

Performance of our Tecnai F30:

Specimens:Thickness 5 - 300 nm,
diameter 3 mm
Holders:Single tilt low background (+- 40° tilt),
double tilt low background,
double tilt low background with cooling (liquid N2),
double tilt rotation holder,
in-situ straining holder,
in-situ STM holder
Resolution:Point res. 0.19 nm,
Information limit 0.12 nm
Magnification:70 x - 18 Mill. x
STEM:Resolution 0.2 nm (Mag. up to 230 Mill. x)
BF-, DF-, HAADF-detectors
EDXS:Lateral resolution < 2 nm. Detection of all chemical elements with Z >= 5 (Bor), detection limit 0.5 %, correctness 20 %
EELS:Lateral resolution < 1 nm. Energy resolution < 1 eV. Especially effective for light elements (e.g. B, C, N, O), detection limit very matrix dependent, >= 0.5 %, correctness 30 %
Energy filtered imaging:Lateral resolution < 1 nm, energy resolution about 1 eV.

 

TEM CM 20 FEG

(200kV, FEG, TEM/STEM, PEELS, EDX, BF/DF, CCD)

Our transmission electron microscope CM20 FEG (from Philips)

Operates at 200 kV accelerating voltage and is equipped with:

  • Field emission gun (FEG)
  • Twin objective lens
  • Scanning unit (STEM) with bright field and dark field detector
  • Energy dispersive X-ray spectrometer (EDXS) (Noran Voyager IIa)
  • Electron energy-loss spectrometer (Gatan PEELS 666)
  • TV-rate camera (TVIPS FastScan F114NX)
  • Secondary electron detector
  • Various specimen holders e.g. for heating, cooling, straining

 

FIB Helios 5 CX

Focussed Ion Beam Microscope (FIB)

The Focussed Ion Beam (FIB) technology (FIB Helios 5 CX, ThermoScientific) is used for investigations in materials research or microelectronics, esp. for high contrast imaging of thin film microstructure using the channeling effect, cross section preparation, failure analysis, microstructuring, or thin film device modification. Using a focussed Gallium ion beam, it can precisely remove or deposit material at the sample surface on a submicron scale as well as image the sample surface or cross-section producing high quality contrast images with high magnifications.

SEM Zeiss Ultra Plus

(FEG, EDX, WDX, EBSD)

Our SEM Ultra Plus (Zeiss) is a high-resolution SEM with:

  • FEG source (Schottky type)
  • EDX  for elemental analysis with peltier cooled Si(Li) detector (Oxford Instruments)
  • WDX  for elemental analysis (Oxford Instruments)
  • EBSD system Symmetry S3 (Oxford Instruments) for local orientation analysis
  • Gas injection charge compensation system

Special characteristics of the system:

  • primary energy 0.02 - 30 keV, beam current 12 pA to 40 nA
  • Complete detection system with ESB, Inlens, AsB, and Everhart Thornley detector
  • Insensitive to charging effects, gas injection charge compensation system
  • Various TEM specimen holders (heating, LN2 cooling, double tilt rotation, cooling-straining, and in-situ TEM-STM)
  • Micromanipulators MM3 with RoTip and Gripper for FIB or SEM
  • TEM in-situ STM with Nanofactory STM Holder

Surface Analysis

XPS PHI 5600-CI

(Physical Electronics)

The XPS system enables quantitative element analysis at surfaces of solid materials by spectroscopy of emitted photo electrons and gives information on the chemical states by analysis of peak-shifts or peak-shape changes.

System characteristics:

  • excitation by Al-Ka (1586.6 eV) or Mg-Ka (1253,6 eV) X-rays, monochromatized Al-Ka, or He-UV-radiation
  • electron analysis with a 150 mm diameter hemisperical energy analyzer with 16-channel multi-channelplate detector, pass energy from 2.9 to 175 eV, best energy resolution at Ag3d = 0.8 eV
  • local analysis (best in the region of 100 µm) by a special lens-system, automatic map- and line-scan-analysis by a scanning system up to 2 mm * 2 mm, typical analysis region of 800 µm diameter
  • sample holder 1 and 2 inch, computer-controlled sample tilt for automatic angle-resolved measurements
  • sputtering with a SPECS IQ 12-38 ion gun typically by noble gas ions (e.g. Ar+) for surface cleaning and depth profiling, 2 mm * 2 mm scan region, 1 ... 4 nm / min sputtering rate
  • low energy electron flood gun for charge compensation
  • UHV vacuum system with a combination of Ti ion getter and an Ti sublimation pump, base pressure 10-8 Pa (10-10 Torr), fast load lock pumped with a turbomolecular pump, sample transfer between XPS and AES (and with glove box) without air exposure (p < 10-5 Pa) possible
  • UHV-coupling with 2 preparation chambers (heating, evaporation, scraping, sputter deposition)

Auger Microprobe JEOL JAMP 9500F

Features

  • automatic UHV vacuum system, pressure typical 5*10-7 Pa
  • fast sample transfer (5 min)
  • automated sample stage with probe tracking function

Excitation Source

  • Field emission electron gun, ~20 nm min. spot size for Auger analysis, 3…30 keV primary energy
  • 1 pA... 200 nA electron current, typical for Auger analysis: 10keV, 10 nA

Detection System

  • hemispherical analyser energy range 0…2500 eV
  • CRR mode: retarding ratio = 0.32 (normal mode) ... 0.02 (high resolution)
  • constant pass energy mode (CAE) for XPS analysis
  • 7 channel detector with open channeltrons
  • secondary electron detector with scintillator system

Sputtering System

  • differentially pumped ion gun 500…3000 eV (sputter gas: mainly Ar)
  • low energy ion production for charge neutralization possible
  • (compucentric) sample rotation to minimize ion beam induced roughening during sputtering

Additional Capabilities:

  • in-situ impact fracture stage for analysis of grain boundaries and other internal surfaces
  • EDX system QUANTAX 400 for quantitative micro analysis
  • transfer chamber for sample transport in noble gas atmosphere from glove-box
  • X-ray source (SPECS Al- Mg-anode, non monochromatic) for XPS analysis, local spatial resolution in 2-mm-range by use of a collimator

Software for analysis in electron spectroscopy

  • PHI MultiPak®: software for evaluation AES spectra and maps (Physical Electronics)
  • pca_men: Matlab® based package of routines for factor analysis of electron spectra (IFW)
    Download of a manual is possible here (hitherto German version only: Handbuch Deutsch).
  • pca_image: Matlab® based package of routines for factor analysis of elemental maps (IFW)

Combined SIMS/XPS PHI6300/Phoibos 100MCD

  • System based on a PHI 5600 vacuum vessel from EUROVAC, equipped with the SIMS component PHI 6300 (Physical Electronics) computerized by a solution of RBD Enterprises and the XPS system PHOBOS 100 (SPECS).
  • Pumped by a combination of a Ti ion getter pump and a Ti sublimation pump, base pressure 10-7 Pa, fast load lock for 1 inch sample holders compatible with the PHI-system.
  • Sample inspection with an optical zoom microscope.

SIMS

  • trace element analysis with mass spectrometry of secondary ions produced by ion beam bombardment
  • primary ions from a microfocus (5 ... 30 nm diameter depending on element) ion column, scan up to 3 mm * 3 mm, ions O2+, Ar+ (Duoplasmatron), or Cs+ (evaporation source) 1.5 to 5 keV
  • mass analysis with a quadrupol-mass analyzer (BALZERS 1....255 u) with electrostatic sector field, ion detection with channeltron
  • dynamic range 1 to 106 counts/s, electronic gate selectable in area
  • charge compensation with an electron gun (SPECS)
  • simple function for elemental mapping: automatic conversion to bmp files with 256 steps
  • Analytical features

XPS

  • quantitative element analysis at surfaces of solid materials by spectroscopy of emitted photo electrons, information of the chemical states by analysis of peak-shift or peak-shape changes
  • excitation by Al-Ka or Mg-Ka X-rays (300 W)
  • electron analysis with a 100 mm diameter hemisperical energy analyzer with 5-channel multi-channelplate detector, pass energy variable up to 660 eV, best energy resolution at Ag3d = 0.95 eV
  • local analysis (best in the region of 300 µm) by a special lens-system, different analyzer modes in area and transmission properties, also for LEIS, UPS, ISS
  • sputtering with a SPECS IQ 12-38 ion gun typically by noble gas ions (e.g. Ar+) for surface cleaning and depth profiling, 3 mm * 3 mm scan region, 1 nm / min sputtering rate
  • analysis of non-conducting samples, additional electron flood gun
  • possibility of surface investigation by light ion scattering (ISS) with the SPECS ion gun, low-sophisticated Auger analysis possible (W-cathode, 0.1 mm beam size)
  • UHV-coupling with preparation chambers possible (same system as PHI 5600 CI)

Materials Preparation and Film Deposition

Cluster tool Creavac Creamet 350 CI 6 ("CARMEN")

CARMEN is a Clustertool for Advanced Research on Thin Film Materials for Electroacoustic Nonconventional Devices

The deposition machine CARMEN is a versatile tool for various deposition techniques.

Description of the tool:

Chamber in the middle = handler for transfer and with three measurement stages (optical layer thickness, electrical sheet resistance method in construction)
Chamber 1 = load lock with hot carrier system (heating in all chambers except chamber 6)
Chamber 2 = ion beam pretreatment (Mark I+ Kaufman-type ion source) for surface preclean and etch applications with high-current, low-energy ions
Chamber 3 = DC magnetron co-sputtering of metallizations (Cu, Al, Ag, Ti, W, Co, Fe, Ni, Zr)
Chamber 4 = HF magnetron sputtering (reactive) of metallizations and barriers (Ti, Ru, Ta5Si3, TaSiN)
Chamber 5 = HF magnetron sputtering (reactive) of insulators (SAW-grade SiO2)
Chamber 6 = e-beam evaporation (Cu, Al, Ag, Au, Ti)

  • base pressure 10-6 mbar down to low 10-7 mbar
  • dry vacuum system (roots and turbo molecular pumps)
  • controlled carrier heating RT to 500°C and cooling (ramps 2 to 20 K/min)
  • computer controlled processing and monitoring
  • inspection/process flow via Internet
  • Local Deposition by Electrons & Ions (EBID & IBID in FIB)

Testing of Microelectronic Devices

  • Measuring systems for low electrical resistance

Specimen Preparation

Focussed Ion Beam Helios 5 CX

(From Thermo Scientific)

The Focussed Ion Beam (FIB) technology (FIB Helios 5 CX, Thermo Scientific) is used for investigations in materials research or microelectronics, esp. for high contrast imaging of thin film microstructure using the channeling effect, cross section preparation, failure analysis, microstructuring, or thin film device modification. Using a focussed Gallium ion beam, it can precisely remove or deposit material at the sample surface on a submicron scale as well as image the sample surface or cross-section producing high quality contrast images with high magnifications.

Focussed Ar-ion thinning with NanoMill 1040

(From Fischione)

Broad beam ion thinners

RES 101 (BAL-TEC)
BAL-TEC RES 010 Special Low Energy
RES 010 (BAL-TEC)
PIPS 691 (Gatan)
PIPS 691 LN2 cooling (Gatan)

Wafer saw DAD 3220

(Disco)

Wire saw, grinding, polishing, and dimpling machines, ultrasonic cutter

Electrolytic thinning with TenuPol-5

at low temperatures (-70°C)

(Struers)

Plasma cleaner TPS 216

(Binder Labortechnik)

for removing contamination and ultra-low energy thinning with special sample holder

Micropipette Puller PC-10

(Narishige)

Data Analysis and Modelling

  • Analysis of Microstructures
  • 3D-Reconstruction
  • COMSOL - Multiphysics
  • Programming systems:
  • Materials Properties Database
  • Software for image simulation and analysis in electron microscopy
    • ELDISCA: Windows(TM) based software for evaluation of (point and ring) diffraction patterns.
    • Simulation of electron microscopic images and spectra: Java-EMS, Fortran/C-EMS (P. Stadelmann/EPFL), IdealMicroscope (EMLab Software), FEFF8 (University of Washington)
    • Image analysis: DigitalMicrograph (Gatan), IDIM (Iterative Digital Image Matching, according Research Paper) for the analysis of HRTEM images
    • Exit-wave-reconstruction: TrueImage (Thermo Fisher Scientific, formerly FEI Company, formerly Philips Electron Optics)
    • Construction and visualization of crystal structures: CrystalKit (Total Resolution) for interfaces, CrystalMaker (CrystalMaker Software) for crystals
  • ARXPS Analysis and Simulation
  • pca_men: Matlab® based package of routines for factor analysis of electron spectra (AES, XPS, EELS).
    Download of a manual is possible here (hitherto German version only: Handbuch Deutsch).