Broad Argon Beam Tools for SEM Prep -...

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CONFIDENTIAL (presentation title here) Broad Argon Ion Beam Tools for SEM Prep Mike Hassel Shearer 1 & Vikstrom Hakan 2 1 Gatan 2 Oxford Instruments
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Transcript of Broad Argon Beam Tools for SEM Prep -...

  • CONFIDENTIAL (presentation title here)

    Broad Argon Ion Beam Tools for SEM Prep

    Mike Hassel Shearer1 & Vikstrom Hakan2 1 Gatan

    2 Oxford Instruments

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    Commercial Slide

    Ilion II- Argon Prep Tool

    Murano in-situ EBSD Heating Stage

    Oxford Instr. Nordlys EBSD System

    MonoCL4- Cathodoluminescence

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    Why Is Sample Prep Important & Requires Intuitive Skill ?

    FIB + 300 V Argon Polish

    Argon Polish 8Kev + 1 KeV

    Argon Polish 6 KeV

    Titan TEM Image of Transistor Gate

    SEM Image FOV 500 micron in diameter ready for EBSD

    SEM Image FOV 1mm x 600 microns voids as small as 4nm visible . Key analysis in Fracking

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    Some of the Tools Used for Sample Prep.

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    Or Even These $$$$$ ! Useful ? Not Always

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    Work Flow: From Bumper to Microstructure --- How ?

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    Argon Polish 6Kev + 1 KeV

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    WorkFlow for Steel and Hard Materials

    Outcome:

    Large Polished/Undamaged surface to use for grain size and grain orientation analysis in test samples or structural components.

    This means using a SEM ( Back-Scattered Image) and EBSD.

    Often this work to be done at elevated temperature (Murano).

    Issues:

    Large Area >500 micron x 500 microns restricts the use of FIB

    Mechanical Polish requires skill and every material may require a special process. Additionally the process may require the use of chemicals (acids) to remove final damage layer.

    Solution:

    Broad Argon Beam Tool (Ilion II) in both cross section or planar mode.

    Murano for in-Situ EBSD at Temperature

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    Mechanical Polishing Steps for a Specific Hardened Steel

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    STEP PG FG DP1 DP 1B DP2 DP3 OP

    Surface SiC Paper 320 MD-Largo MD-Dur MD-Dur MD- Nap MD-Nap MD_Chem

    Suspension

    DiaPro Allegro

    9 micron

    DiaPro Dur 3

    micron

    DiaPro Dur 3

    micron

    DiaPro Nap B 1

    micron

    DP-Susp.P 1/4

    micron OP-AA

    Lubricant Water Blue Lub

    rpm 300 150 150 150 150 150 150

    Force (N) 30 30 30 15 10 10 10

    Time (min) 1 5 to 10 5 5 5 5 5

    Hardened Steel

    Source : www.ebsd.com ( very useful Website)

    Hardened steels The distorted lattice of martensite makes it difficult to get a good quality EBSD. Good results are obtained on hardened plain carbon and low alloy steels containing various amounts of martensite using a long fine diamond polishing process. Alumina (OP-AA) is preferred for final polishing to obtain a proper final result with a minimum amount of relief. The result obtained for a tool steel (9CrWmn)

    http://www.ebsd.com/

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    Mechanical Polish Workflow

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    Saw Grind & Polish Acids & Cleans

    Experience and Luck

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    Ilion II Workflow

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    Cut to correct size Polish to 9 microns

    Ilion II

    Advantages of Ilion II vs. Mechanical/Chemical Polish: • Material Neutral • No Experience Base required • No Acid/Chemicals used

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    Ilion II Cross Section Process ( 8keV 2hr. + 1keV 30 min.)

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    Ilion II Blade

    9 micron diamond polish then Ilion II . No chemical etch to bring on the grain structure

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    BSE Image Near Polish-Non Polished Interface

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    BSE Image from central region (~200 micron x 200 micron)

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    Retained austenite in martensite steel

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    EBSD analysis

    IPF

    Phases map

    Martensite retained Austenite (9%)

    IPF map

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    Affect of Argon Polishing Voltage on EBSD Results

    see www.srim.org for details of the effect of Noble Ion Species on Sputtering ( yields, implant, damage) at LOW Voltage

    http://www.srim.org/

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    Ilion 8keV, 122μA, 5 min

    Tungsten Carbide NO Phase transformation of the Co Phase to Hex unlike prep with FIB

    WC WC Co (fcc)

    Ilion II Polishing of W-Carbide with Cobalt Phase

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    Argon Milling W-Carbide Compare to 8 KeV

    MC4: Improved EBSD indexing

    Gallium Ion beam milling damage degrades the EBSD patterns leading to poor indexing. By milling using broad Ar ion beam (Ilion) we can obtain better EBSD quality so that the patterns can be indexed automatically.

    Illion 1keV, 28µA, 120 min

    WC WC Co (fcc)

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    Sample 1

    Cross section

    AZtec user interface showing data as acquired i.e. raw data; both EDS and EBSD were acquired simultaneously.

    Sample 1 Cross Section Al2O3/TiCN/WCarbide

    Aztec guides the user through the set up and acquisition process, and is extremely intuitive and easy to use.

    • EBSD allows a wide raft of measures, plots and maps to be obtained, and is highly complementary with EDS, a combined system provides a full analysis of the microstructure, texture, phases and chemistry amongst other advanced measures

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    Band contrast map showing a greyscale image derived from the quality of the Electron Backscatter Patterns (EBSPs); lighter shades are indicative or higher quality patterns and vice versa. This type of map can reveal fine structures and detail not visible in the electron image(s)

    Sample 1 Polished at 6KeV 90 minutes + 1 KeV 60 minutes

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    Inverse Pole Figure (IPF) colour coded map for all phases

    IPF colour keys for WC, TiCN, Al2O3, left to right, showing the orientation relationship with respect to colour for each of the phases.

    Sample 1

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    Showing strong alignment of Al2O3 crystals (note position of cursor (cross) in each image) resulting from and indicative of the growth dynamic

    Sample 1

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    EBSD in-Situ at Elevated Temperature

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    525 Murano Heating Stage

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    Model 525 – Murano Heating Stage

    Temperature range up to 950 °C , accuracy

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    Application : Identification - Phase transformation

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    300 µm

    In-situ phase transformation observed in low carbon steel

    945 °C

    Specimen heated to 945 °C full transformation to Austenite phase Austenite FCC Ferrite BCC

    Data courtesy – Oxford Instruments (Dr. Singh Uhbi)

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    Ferrite BCC

    300 µm

    In-situ phase transformation observed in low carbon steel

    945 °C 0 mins 895 °C 5 mins

    Murano temperature control allows transformation to Ferrite phase to be mapped.

    Austenite FCC

    Data courtesy – Oxford Instruments (Dr. Singh Uhbi)

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    Austenite FCC Ferrite BCC

    300 µm

    In-situ phase transformation observed in low carbon steel

    945 °C 0 mins 895 °C 5 mins 895 °C 10 mins

    Murano stable temperature control allows transformation to Ferrite phase to be mapped.

    Data courtesy – Oxford Instruments (Dr. Singh Uhbi)

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    Austenite FCC

    300 µm

    In-situ phase transformation observed in low carbon steel

    945 °C 0 mins 895 °C 5 mins 895 °C 10 mins 880 °C 15 mins

    Additional controlled cooling to 880°C observe nearly full transformation to Ferrite phase Ferrite BCC

    Data courtesy – Oxford Instruments (Dr. Singh Uhbi)

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    In-situ phase transformation observed in low carbon steel

    Data courtesy – Oxford Instruments (Dr. Singh Uhbi)

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    LED’s Broad Argon Ion Beam + Cathodoluminescence

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    LEDs and solar materials – ‘exotic’ semiconductors Although these are semiconductor materials they are not ‘Semi’

    Silicon for Semi is the most perfect material ever created

    Zero dislocations or grain boundaries in 300mm diameter wafer

    1 in 1 Billion atoms ‘incorrect’

    Why the need for this ‘perfection’? Defects kill devices

    Why don’t we use silicon for LEDs?

    It is fundamentally inefficient at emitting light (and absorbing sun rays)

    o World record LED efficiency for silicon = 0.00005%

    o Maximum PV efficiency for silicon = 33.7%

    So we look for other materials that are ‘right’

    LEDs: GaN, GaP, InP, ZnO, CdZnTe, …..

    PV: CIGS, CdTe/CdS, Ge, triple junction, ……..

    But these are all difficult to grow and contain many defects

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    ‘Exotic’ compound semiconductors Doesn’t matter what the latest trendy material is, we (almost) always

    need to understand the same things:

    Composition SEM/TEM, EDS, PIPS II, EELS, CL

    Interfaces SEM/TEM/FIB, Ilion II, EELS

    Electronic band gap SEM/TEM/FIB, PIPS II, Ilion II, EELS, CL

    Grain structure SEM/TEM, PIPS II, Ilion II, EBSD

    Electrical activity of defects PIPS II, Ilion II

    o Grain boundaries SEM/TEM, CL, EBIC

    o Dislocations SEM/TEM, CL, EBIC, C100X

    o Point defects CL, CF302

    Doping SEM/TEM, PIPS II, Ilion II, EELS

    Conversion efficiency: light-to-current or current-to-light (LED) Ilion II CL, EBIC

    Physics Ilion II CL, EBIC, CF302, C100X

    Electric fields Ilion II EBIC

    Stress TEM, CL, PIPS II 34

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    How white LEDs work Convert electrical energy into white light

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    LED Chip

    A

    Phosphor converter

    UV/Blue photon (electroluminescence)

    White light (photoluminescence)

    LED chip Determines raw brightness and efficacy

    Phosphor Determines color

    Packaging

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    LED Chip (green) – current generation

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    Commercially Purchased HB LED – Ilion-milled

    1mm Cut Width

    4hr cut time

    Materials from: Plastic, Sapphire, Phosphor, Gold, Silicone Gel, Silicate

    Great for CL as well

    I count about 20 interface of interest in this one sample

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    Ilion Prep’d LED and EDS

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    RGB CL Image of LED

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    Ultra High Resolution Image of the Active region of the Device

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    Rock 石头 (shitou) ぐう (jan) 위 (bawi) Sten

    Stein

    Kivi

    Paper 布 (bu) ぱー) (pon) 보 (bo). Papper

    Papir

    Paperi

    Scissors 剪刀 (jiandao) ちょき (ken) 가위 (gawi), Sax

    Saks

    Sakset

    Broad Argon Beam Tools Can Cross Section Almost Anything

    Shale Paper Plate W-Carbide

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    Thank You