INSPICO
High Resolution Analysis

REVOLUTIONIZING NANOTECHNOLOGY

Introducing the Hybrid Dual Beam APT Microscope System ORBIS

Nanotechnology is a key technology for the development of various new products and materials. To be able to develop and produce these technologies or to ensure their quality, a special kind of microscopes is necessary. Atom probe tomography (APT) as well as dual beam microscopy (FIB/SEM) are powerful tools in nanotechnology with enormous scientific output. The combination of both techniques is able to deliver information up to sub-nanometer resolution of many material classes. However, sometimes the application becomes limited by the spatial separation of the two techniques. To enable the analysis of liquids and soft matter by APT, we designed a new hybrid instrument which represents a combination of dual beam scanning microscope for FIB preparation and miniaturized APT chamber. The dual beam tool can be extended by all facilities to enable cryo-preparation.


Discovering new possibilities

  1. Standard Protocols: Compatible with established methods like lift-out technique and single tips in metal tubes.
  2. Vacuum Maintenance: Sample preparation and direct measurement without breaking vacuum, ideal for sensitive materials.
  3. Correlative Information: Simplified acquisition of EBSD, EDX, and STEM data on the same sample.
  4. Cryo Samples: Direct APT measurements of samples prepared under cryo conditions are possible.
  5. Tip Inspection: Inspection and reshaping of the sample before and after APT measurements using modern SEM instruments.
  6. Emitter Shape Extraction: Determination of the emitter shape before and after measurement to improve reconstruction quality.
  7. Micro-Tip Preparation: High-precision creation and positioning of micro-tips within the material using SEM.
  8. Electrode Inspection: Checking and refurbishing the microelectrode in the SEM to optimize measurement quality.
  9. Variable Laser Wavelengths: Options for infrared, green, and UV wavelengths for maximum flexibility.
  10. Compact Design: Reduced instrument size to minimize space requirements.



A small side chamber had to be developed and attached to an appropiate FIB port (mostly the Airlock-Port). The chamber is necessary to achieve the necessary UHV conditions for APT. The chamber is amongst other equipped with an MCP based Delay Line Detector (Diameter 80 mm), Cool Head, Hich Voltage Connectors, Laser Ports with associated manipulating optics and transfer mechanics. 

The sample of interest is mounted onto the shuttle



Transfer

  1. Transfer of the shuttle into the FIB chamber
  2. Localisation: The micro stage electrode is rotated backwards to open the view onto the sample. Localisation of the feature of interest
  3. Milling: a) The feature of interest is milled or prepared by Lift Out procedure b) the electrode is machined by the Ion Beam
  4. Positioning: The micro stage electrode is rotated back towards the sample. Using the SEM Beam, the electrode is positioned precisely above the the milled feature.
  5.  Transfer into the M-Tap: The shuttle is transfered back into the side chamber.It is cooled down to croygenic temperatures and aligned relativ to the laser spot. APT measurement is started. 


Samples are mounted directly onto the Shuttle. Using the transfer mechanics the complete shuttle can be transferred directly into the Dual Beam instrument. Allowing direct manipulation of the sample using Dual Beam Techniques.


Optional Airlock Chamber with Cryo Option









Optional Airlock-chamber with Cryo-Option

Pneumatic attachment of the Cooling Unit




 Specs: Orbis - Modular Atom Probe -

Modular  Atom Probe + Sample Shuttle

  • Atom probe shuttle
  • Mobile sample stage with piezo-driven extraction electrode
  • automatic connection to high voltage supply, cooling, and computer control
  • FIB mounting stage for atom probe shuttle
  • 75 mm Delay Line Detector
  • 2-dim Delay-Line-Detector 


OPTION  

  • MCP chevron stack with L/D 80:1  (12.5 micron pore size, 1 mm thick, OAR 70% or 90% active/linear diameter 75mm
  • all required high voltage supplies
  • front-end electronics assembly with improved temporal and spatial resolution
  • multi-hit dead-time 10 ns for  fast signals   
  • constant fraction discriminator   and pulse height analyzer
  • 8-channel TDC based on the CERN HPTDC 
  • <100psec resolution (nominal  least bit 25psec)
  • unlimited range and number of  hits with dead-time of <10 ns
  • High voltage tip supply 0-10 kV with automatic control


Cryo system

  • two-stage Gifford-McMahon Cryo-Head
  • Pmax > 2 W (20 K) 
  • Pmax > 8.5 W (77 K)  
  • Cryocontroller    
  • vibration damping

 

Optical System

  • Piezo driven laser mirror system
  • active alignment during measurement 
  • diameter of laser probe < 10 mm  


Sample Stage

  • Five axis piezo-driven sample  stage

 

Vacuum system

  • UHV single modular chamber design (p < 5x10E-10 mbar)
  • UHV safe transfer between FIB and atom probe chamber  
  • oil-free vacuum
  • pneumatic separation valve and vibration insulation to the FIB instrument  
  • SPS control incl. touchpad to operate   the vacuum
  • Camera-based alignment system  for laser beam 
  • Windows PC incl. double monitor
  • Windows-based front-end software  to operate measurement incl. active control of piezo drives and high voltages


Evaluation software package ‘Scito’

  • full transparency in used algorithms
  • mass spectrum analyser  
  • state-of-the-art volume   reconstruction
  • 1D and 2D composition profiles and mapping
  • 3D iso-concentrations plots
  • cluster search and analysis
  • data I/O tools
  • Statistical testing tools
  • Starting set of spare parts,   basic maintenance tools, complete technical documentation including wiring diagrams and instructions for first problem solving

 

Transfer   Chamber / Airlock on request

  •  UHV chamber with: two  CF-63 flanges for transfer of the atom probe shuttle between FIB and APT, and   a further CV-63 flange to adapt custom process chambers  
  • Oil-free vacuum (turbo molecular pump) background pressure <10-8 mbar, Integration into   central vacuum control unit of the instrument
  • Ion gauge 
  • Cryogenic  cooled storage for up to four sample holders (LN2, dewar) 
  •  Cryo-stage   for the atom probe shuttle 
  • (LN2,   dewar)
  •  Temperature readout


Laser Options

UV Nanochiplaser

  • Pulse time 500 ps
  • Repetition rate: 130 kHz


Picosecond industrial laser (10ps, 6W)

  • Diode-pumped, 1064 nm picosecond industrial laser with a specified power output of > 6 W at 1000 kHz. Includes a controller consisting of a power supply and cooling unit, as well as an additional SHG/THG module.
  • Average power at 355 nm: 1.5 W @ 200 kHz
  • Average power at 532 nm: 1.5 W @ 200 kHz
  • Pulse length: < 15 ps
  • Pulse repetition rate: 0–1000 kHz
  • Beam quality: M² < 1.3


Femtosecond Laser

  • Wavelength: 1030 nm ± 3 nm
  • Pulse Energy: Up to 10 μJ at 500 kHz; 5 μJ at 1 MHz
  • Repetition Rate: Single pulse up to 2 MHz
  • Pulse Width: < 400 fs
  • Mode: TEM00

 

  • Second Harmonic Generation (SHG): 515 nm, efficiency: >50%
  • Third Harmonic Generation (THG): 343.3 nm, efficiency: >15%