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Cryo FIB-TEM sample preparation of plate rolled Zr-2.5%Nb sheets A. Steiger-Thirsfeld a , L. Whitmore a , S. Schwarz a , G. Rumplmair a , K. Whitmore a , R. Hengstler b and J. Bernardi a a Vienna University of Technology University Service Center of Transmission Electron Microscopy Wiedner Hauptstraße 8-10 1040 Wien Wiedner Hauptstraße 8 10, 1040 Wien b AREVA NP G bH b AREVA NP GmbH Paul-Gossen-Straße 100 91052 Erlangen

Cryo FIB-TEM sample preparation of plate rolled Zr-2.5%Nb sheets · 2010. 7. 14. · Cryo FIB-TEM sample preparation of plate rolled Zr-2.5%Nb sheets A. Steiger-Thirsfelda, L. Whitmorea,

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Text of Cryo FIB-TEM sample preparation of plate rolled Zr-2.5%Nb sheets · 2010. 7. 14. · Cryo FIB-TEM...

  • Cryo FIB-TEM sample preparation of plate rolled Zr-2.5%Nb sheets

    A. Steiger-Thirsfelda, L. Whitmorea, S. Schwarza, G. Rumplmaira,K. Whitmorea, R. Hengstlerb and J. Bernardia

    aVienna University of TechnologyUniversity Service Center of Transmission Electron MicroscopyWiedner Hauptstraße 8-10 1040 WienWiedner Hauptstraße 8 10, 1040 Wien

    bAREVA NP G bHbAREVA NP GmbHPaul-Gossen-Straße 10091052 Erlangen

  • Outline

    A li ti f Z ll•Application of Zr alloys•Different methods for preparing TEM samples from rolledZr alloy •Comparison of preparation methods concerning theinduced damageg•Cryo Assembly•Cryo FIB-TEM preparation

  • Application of Zr alloys

    Cladding of fuel rods in nuclear reactors

    Assessment of the Kinetics of Local Plastic Deformation of Zr-2.5%Nb CANDU Pressure Tubes,Talk by Bipasha Bose, Ontario, 2010

    •Zr has a very low absorption cross-section of neutrons•Alloying components for improvement of corrosion resistance•Alloying components for improvement of corrosion resistance

  • Task

    Samples

    Plate rolled Zr-2 5%Nb alloy sheetsPlate rolled Zr-2.5%Nb alloy sheets of 0.33mm thicknessannealed at 580°C in vacuum for 2hours2hours

    TEM sample of the near surface layer (~10μm) with a minimum of preparation damage andfinal sample thickness ≤100nm p

  • Electro-polishing

    Thomson-Rusel, Edington

    TenuPol-5

    Unfortunately this methoddoes not allow preparation of cross-sectionsof cross-sections

  • Wedge shaped grinding

    MultiPrep™ System

    DuoMill

    4kV Argon ions, LN2

  • Ultramicrotome

    Zr has a Mohs hardness of 5

    www.bio.miami.edu

    PowerTome PC

  • FIB at RT

    Quanta 200 3D DualBeam

    5kV cleaning for 2minuteswith Ga ionswith Ga ions

    1kV Ar ions for 1hour0 5kV Ar ions0.5kV Ar ions for 10minutes

    gentle mill

  • Post-ion treatment

    Precision Ion P li hi SPolishing System

    (PIPS)

    4KV Argon ionsfor 10 minutes

  • Quorum PP2000T Cryo Assembly(1)

    SEM cooling ddewar

    Cryo preparation chamber (turbo pumping system located on the floor behind the SEM)

    Controls

    floor behind the SEM)

    Transfer deviceLiquid nitrogen slusher (for rapid sample freezing)sample freezing)

  • Quorum PP2000T Cryo Assembly (2)

    Sample transfer

    Cryo preparation chamber

    Sample transfer device

    y p p

  • Quorum PP2000T Cryo Assembly (3)

    SEM cold stage

  • Cryo-Applications

    Water ice growth on Siat -100°C

    Fracture surface of citric acidin oil emulsion at -100°C

  • Lift out pre-preparation at RT

  • H-bar pre-preparation at RT

  • Sample holder

  • Cryo preparation steps

    •Purging the system for 10-15 minutes with N2 gas flow of4l/min

    •Cooling of the stage with the sample and the cold trap (-190°C)

    T dj ( id h ll ) d•Temperature adjustment (cartridge heater, controller) andstabilizing for about 30min

    R FIB ti t diti ( i 165°C)•Resume FIB preparation at cryo conditions (min. -165°C)

    •Last FIB preparation step: 5kV Ga cleaning at cryo conditionsconditions

  • Difficulties

    •Restricted sample rotation

    •Sample drift through temperature instabilities•Sample drift through temperature instabilities

    •Extended preparation time

    •N2 consumption

  • Results Cryo FIB (lift out)

  • Results Cryo FIB (H-bar)

  • Summary

    •Different methods for preparing TEM samples from Zrp p g p•Low energy ion beams (Ar, Ga) cause damage in Zr at RT•Cryo Assembly

    •Cryo FIB-TEM preparation

    Electro-polishing Cryo FIB preparation

  • Thanks a lot for your attention